WO2012160872A1 - 炭化珪素基板、炭化珪素インゴットおよびそれらの製造方法 - Google Patents

炭化珪素基板、炭化珪素インゴットおよびそれらの製造方法 Download PDF

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Publication number
WO2012160872A1
WO2012160872A1 PCT/JP2012/058527 JP2012058527W WO2012160872A1 WO 2012160872 A1 WO2012160872 A1 WO 2012160872A1 JP 2012058527 W JP2012058527 W JP 2012058527W WO 2012160872 A1 WO2012160872 A1 WO 2012160872A1
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Prior art keywords
silicon carbide
region
ingot
substrate
nitrogen
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English (en)
French (fr)
Japanese (ja)
Inventor
佐々木　信
太郎 西口
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Priority to CN2012800193499A priority Critical patent/CN103476975A/zh
Priority to DE112012002192.4T priority patent/DE112012002192T5/de
Publication of WO2012160872A1 publication Critical patent/WO2012160872A1/ja
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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
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C30B23/025—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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/21—Circular sheet or circular blank
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24273—Structurally defined web or sheet [e.g., overall dimension, etc.] including aperture
    • Y10T428/24322—Composite web or sheet

Definitions

  • the present invention relates to a silicon carbide substrate, a silicon carbide ingot, and a method of manufacturing the same, and more particularly to a silicon carbide substrate, a silicon carbide ingot, and a method of manufacturing the same with less variation in characteristics such as impurity concentration.
  • silicon carbide has been studied as a next-generation semiconductor material to replace silicon (Si).
  • SiC silicon carbide
  • a method of growing a silicon carbide single crystal on a seed substrate to form a silicon carbide ingot, and slicing the silicon carbide ingot to manufacture a substrate In this case, a seed crystal is prepared with a (0001) plane (so-called c plane) or a crystal plane with an off angle of 10 ° or less from the c plane as a growth plane, and a silicon carbide single crystal is formed on the seed crystal growth plane.
  • a growing method is used (see, for example, Japanese Patent Application Laid-Open No. 2004-323348 (hereinafter referred to as Patent Document 1)).
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2004-323348
  • Patent Document 1 in order to prevent the formation of heteromorphic crystals and differently oriented crystals and to prevent the generation of screw dislocations, a dislocation control seed crystal having a region capable of generating screw dislocations is prepared, and A silicon carbide single crystal is grown. Further, in Patent Document 1, in the growth step of the silicon carbide single crystal, a c-plane facet is formed on the surface of the silicon carbide single crystal, and the (0001) facet and the region capable of generating screw dislocation partially overlap. To grow a silicon carbide single crystal. According to Patent Document 1, it is possible to suppress the formation of heteromorphic crystals and differently oriented crystals in the silicon carbide single crystal and the generation of screw dislocation by growing the silicon carbide single crystal as described above.
  • the (0001) facet is overlapped with the region capable of screw dislocation generation by controlling the concentration distribution of the reaction gas or controlling the temperature distribution of the seed crystal in the growth step of the silicon carbide single crystal. It is suggested to adjust the position of the surface.
  • nitrogen (N) is more easily taken in at the time of crystal growth than at other portions of the surface. Therefore, at the time of the growth of the silicon carbide single crystal described above, a high concentration nitrogen region in which the nitrogen concentration is higher than other regions is formed in the portion under the surface where the (0001) facet is formed. Since the nitrogen concentration in silicon carbide affects the properties such as conductivity and light transmission of silicon carbide single crystal, it is desirable that the ingot and the substrate formed from the ingot be as uniform as possible.
  • the present invention has been made to solve the problems as described above, and it is an object of the present invention to provide a silicon carbide substrate excellent in uniformity of characteristics, a silicon carbide ingot, and a method of manufacturing them. is there.
  • the inventors have completed the present invention as a result of intensive studies on crystal growth of silicon carbide. That is, as the base substrate (see substrate), the inventor set the off angle in the predetermined direction (off angle direction) to the (0001) plane to 0.1 ° to 10 °, preferably 1 ° to 10 °.
  • the (0001) facet formed on the growth surface of the growing silicon carbide single crystal can be formed at the end of the growth surface, and the (0001) facet can be formed sufficiently smaller than the planar size of the base substrate. I found it.
  • the method for manufacturing a silicon carbide ingot according to the present invention is an off-angle direction which is either the ⁇ 11-20> direction or the ⁇ 1-100> direction with respect to the (0001) plane.
  • a base substrate made of single crystal silicon carbide and having a corner of 0.1 ° to 10 °, more preferably 1 ° to 10 °, and growing a silicon carbide layer on the surface of the base substrate
  • a region having a (0001) facet is formed on the surface of the grown silicon carbide layer.
  • a region having a relatively high nitrogen concentration (a high concentration nitrogen region located below the (0001) facet surface) Can be placed at the end of the silicon carbide ingot. Therefore, the region having a relatively low nitrogen concentration (the region other than the high concentration nitrogen region) can be formed as a region including the central portion of the silicon carbide ingot. Therefore, when the silicon carbide substrate is cut out from the ingot, it is possible to easily obtain a silicon carbide substrate in which a region having a relatively low nitrogen concentration is formed in a wide region including the central portion of the substrate.
  • a region with a relatively low nitrogen concentration (a region with a low nitrogen concentration and a stable nitrogen concentration) can be formed in a wide region including the central portion of the substrate, a semiconductor element is formed on the substrate surface.
  • the semiconductor element can be efficiently formed.
  • the nitrogen concentration around the high concentration nitrogen region on the surface of the silicon carbide substrate The low region (low concentration nitrogen region) is enclosed. Therefore, when forming a device on the surface of a silicon carbide substrate, when attempting to form the device in a region having a relatively low nitrogen concentration, the high concentration nitrogen region is avoided to form the device (that is, high concentration) There is a problem that the utilization efficiency of the substrate is lowered because the device is formed avoiding the nitrogen region and the boundary region between the high concentration nitrogen region and the low nitrogen concentration region.
  • the high concentration nitrogen region is disposed at the end of the silicon carbide substrate, the low concentration nitrogen region is formed at the center of the surface of the silicon carbide substrate. Then, since the devices can be formed in a concentrated manner in the low concentration nitrogen region, the substrate can be effectively used.
  • a silicon carbide ingot according to the present invention is manufactured using the above-described method for manufacturing a silicon carbide ingot.
  • the region having a relatively low nitrogen concentration (the region other than the high concentration nitrogen region) can be formed as a region including the central portion of the silicon carbide ingot. Therefore, by cutting out the silicon carbide substrate from the silicon carbide ingot, it is possible to easily obtain a silicon carbide substrate in which a region having a relatively low nitrogen concentration is formed in a wide region including the central portion of the substrate.
  • a method of manufacturing a silicon carbide substrate according to the present invention includes the steps of preparing a silicon carbide ingot using the above-described method of manufacturing a silicon carbide ingot, and slicing the silicon carbide ingot.
  • the region having a relatively low nitrogen concentration (region other than the high concentration nitrogen region) can be formed as a region including the central portion of the silicon carbide ingot. Therefore, in the step of slicing, a silicon carbide substrate having a region relatively low in nitrogen concentration formed in a wide region including the central portion of the substrate can be easily obtained by cutting out the silicon carbide substrate from the silicon carbide ingot. it can.
  • the silicon carbide substrate according to the present invention is manufactured using the above-described method for manufacturing a silicon carbide substrate. In this way, it is possible to easily realize a silicon carbide substrate in which a region having a relatively low nitrogen concentration is formed in a wide region including the central portion of the substrate.
  • the off angle in the off angle direction which is either the ⁇ 11-20> direction or the ⁇ 1-100> direction with respect to the (0001) plane, is 0.1 ° or more Providing a base substrate made of single crystal silicon carbide at 10 ° or less, more preferably 1 ° or more and 10 ° or less, and growing a silicon carbide layer on the surface of the base substrate; In the step of growing, when considering the crossing angle at which the ⁇ 0001> direction axis of the base substrate crosses the surface of the base substrate in the off angle direction, the upstream end that is the side where the crossing angle becomes an acute angle Forming a region having a (0001) facet on the surface of the grown silicon carbide layer.
  • the portion located under the region having the (0001) facet is a portion other than the portion located under the region having the (0001) facet in the silicon carbide layer
  • the transmittance per unit thickness of light having a wavelength of 450 nm or more and 500 nm or less is further reduced.
  • the (0001) facet that is easily incorporated with nitrogen at the end of the ingot by forming the (0001) facet that is easily incorporated with nitrogen at the end of the ingot, the light transmittance due to the nitrogen incorporated from the facet during growth of the silicon carbide layer is increased. Since the reduced area is disposed at the end of the ingot (the part under the (0001) facet surface), the other part including the central part of the silicon carbide ingot has a relatively high light transmittance. be able to. Therefore, when the silicon carbide substrate is cut out from the ingot, it is possible to easily obtain a silicon carbide substrate in which the region having a relatively high light transmittance is formed in a wide region including the central portion of the substrate.
  • a relatively high light transmittance region (a region with stable nitrogen concentration and transmittance with little incorporation of nitrogen) can be formed in a wide region including the central portion of the substrate, so that the semiconductor element is formed on the substrate surface.
  • the semiconductor element can be efficiently formed.
  • the off angle in the off angle direction which is either the ⁇ 11-20> direction or the ⁇ 1-100> direction with respect to the (0001) plane, is 0.1 ° to 10 °.
  • a base substrate made of single crystal silicon carbide, and a silicon carbide layer formed on the surface of the base substrate.
  • a region having a (0001) facet surface is formed on the surface of.
  • the portion located below the region having the (0001) facet is more nitrogen-rich than the portion located above the region having the (0001) facet on the silicon carbide layer
  • the high concentration nitrogen region may be high.
  • a region having a relatively high nitrogen concentration (a high concentration nitrogen region located below the (0001) facet surface) Can be placed at the end of the silicon carbide ingot. Therefore, the region having a relatively low nitrogen concentration (the region other than the high concentration nitrogen region) can be formed as a region including the central portion of the silicon carbide ingot. Therefore, when the silicon carbide substrate is cut out from the ingot, it is possible to easily obtain a silicon carbide substrate in which a region having a relatively low nitrogen concentration is formed in a wide region including the central portion of the substrate.
  • a region with a relatively low nitrogen concentration (a region with a low nitrogen concentration and a stable nitrogen concentration) can be formed in a wide region including the central portion of the substrate, a semiconductor element is formed on the substrate surface.
  • the semiconductor element can be efficiently formed.
  • the silicon carbide substrate according to the present invention is obtained by slicing the silicon carbide ingot. In this way, it is possible to easily obtain a silicon carbide substrate in which a relatively low nitrogen concentration region (or a region with high light transmittance) is formed in a wide region including the central portion of the substrate.
  • the silicon carbide substrate according to the present invention is obtained by slicing the silicon carbide ingot after removing the high concentration nitrogen region from the silicon carbide ingot. In this way, the high concentration nitrogen region (region with low light transmittance) is removed in advance, so that the region with lower nitrogen concentration than the high concentration nitrogen region (region with high light transmittance than the high concentration nitrogen region) A silicon carbide substrate is formed using the silicon carbide ingot which has become only. For this reason, it is possible to obtain a silicon carbide substrate in which fluctuations in nitrogen concentration and light transmittance are reduced.
  • the nitrogen concentration is relatively higher at one end in either the ⁇ 11-20> direction or the ⁇ 1-100> direction than in the other part.
  • a concentration nitrogen region is formed.
  • the ⁇ 0001> direction axis of the silicon carbide substrate is either with respect to the ⁇ 11-20> direction or the ⁇ 1-100> direction (off angle direction) with respect to the surface of the silicon carbide substrate. It may be formed at the upstream end which is the side where the crossing angle is the acute angle when considering the crossing angle at which it intersects. In this manner, when growing a silicon carbide ingot for forming a silicon carbide substrate, the high concentration nitrogen region is easily disposed at the end of the silicon carbide substrate by controlling the disposition of the (0001) facets. It can be done.
  • the present invention it is possible to obtain a silicon carbide ingot and a silicon carbide substrate excellent in uniformity with respect to characteristics such as nitrogen concentration.
  • FIG. 1 is a schematic plan view of a silicon carbide ingot according to the present invention.
  • FIG. 5 is a schematic sectional view taken along line VV shown in FIG. 4;
  • FIG. 6 is a schematic plan view showing a silicon carbide substrate cut out from the silicon carbide ingot shown in FIGS. 4 and 5.
  • FIG. 1 is a schematic plan view of a silicon carbide ingot according to the present invention.
  • FIG. 5 is a schematic sectional view taken along line VV shown in FIG. 4;
  • FIG. 6 is a schematic plan view showing a silicon carbide substrate cut out from the silicon carbide ingot shown in FIGS. 4 and 5.
  • It is a cross-sectional schematic diagram of the crystal growth apparatus for implementing the film-forming process shown in FIG. FIG.
  • FIG. 5 is a schematic plan view showing another example of the silicon carbide substrate according to the present invention. It is a plane schematic diagram which shows the 1st modification of the silicon carbide ingot according to this invention.
  • FIG. 10 is a schematic plan view showing a silicon carbide substrate cut out of the silicon carbide ingot shown in FIG. 9;
  • FIG. 11 is a schematic plan view showing a modification of the silicon carbide substrate shown in FIG. 10.
  • FIG. 13 is a schematic plan view showing a silicon carbide substrate cut out of the silicon carbide ingot shown in FIG. 12.
  • FIG. 14 is a schematic plan view showing a modification of the silicon carbide substrate shown in FIG. 13.
  • FIG. 13 is a schematic plan view showing a silicon carbide substrate cut out of the silicon carbide ingot shown in FIG. 12.
  • FIG. 18 is a schematic plan view showing a third modification of the silicon carbide ingot according to the present invention.
  • FIG. 16 is a schematic plan view showing a silicon carbide substrate cut out of the silicon carbide ingot shown in FIG. 15;
  • FIG. 17 is a schematic plan view showing a modification of the silicon carbide substrate shown in FIG. 16.
  • FIGS. 1-10 A method of manufacturing a silicon carbide ingot and a silicon carbide substrate according to the present invention will be described with reference to FIGS.
  • a preparation step (S10) is performed.
  • a support member 2 as shown in FIG. 3 is disposed in a processing vessel of a crystal growth apparatus for forming an ingot, and a base which is a seed substrate for forming an ingot on the support member 2.
  • the substrate 1 is mounted.
  • the planar shape of the base substrate 1 is circular.
  • the main surface of base substrate 1 is a silicon carbide (SiC) substrate in which the off angle with respect to the (0001) plane is set to 0.1 ° or more and 10 ° or less, more preferably 0.5 ° or more and 8 ° or less. is there.
  • the film forming step (S20) is performed. Specifically, silicon carbide is formed on surface 4 of base substrate 1 using a sublimation reprecipitation method or the like while heating base substrate 1 after setting the pressure and atmosphere inside the processing container of the crystal growth apparatus under predetermined conditions. Grow a single crystal. Thus, an ingot 10 of silicon carbide as shown in FIGS. 3 to 5 is formed. Further, in the film forming step (S20), the (0001) facet 5 (hereinafter also referred to as the facet 5) is formed on the surface of the ingot 10. The process conditions of the film forming step (S20) are set such that the facets 5 are arranged at one outer peripheral end when viewed from the upper surface of the ingot 10 as shown in FIG. The process conditions will be described later.
  • the nitrogen concentration is relatively higher than in the other regions due to the higher nitrogen uptake from the facet 5 than in the other regions.
  • the high concentration nitrogen region 6 has become high. That is, at the time of growth of silicon carbide constituting ingot 10, relatively more nitrogen is taken into silicon carbide from facets 5 on the surface of the grown silicon carbide than in the other areas, so that high concentration nitrogen region 6 The nitrogen concentration is relatively higher than the nitrogen concentration in the low concentration nitrogen region 7, which is another region.
  • the facet 5 is located at the end in the off-angle direction indicated by the arrow 26.
  • any method can be used.
  • the growth outermost surface of ingot 10 grown on the surface of base substrate 1 base substrate 1 in ingot 10 of FIG.
  • the surface opposite to the side where it is located or the surface of ingot 10 facing the supply direction of the source gas shown by arrow 13 in FIG. 7 is always flat (the surface of base substrate 1 and the growth top surface of ingot 10 are Grow the ingot 10 so that it becomes parallel).
  • the main surface (the surface on which the crystal to be ingot 10 is grown) is in the ⁇ 11-20> direction or the ⁇ 1-100> direction with respect to the (0001) plane. It is preferable to be inclined at 1 ° to 10 °. The inclination angle of the main surface may be 0.1 ° or more and 10 ° or less.
  • a (0001) facet 5 is generated at the end of the ingot 10 as shown in FIG. 7.
  • the support member 2 shown in FIG. 3 is not described, and the base substrate 1 is disposed directly on the inner wall of the crucible 11, but as shown in FIG.
  • the support member 2 may be disposed on the base substrate 1, and the base substrate 1 may be fixed on the inner wall of the crucible 11 via the support member 2.
  • the growth outermost surface of the ingot 10 is made as flat as possible (for example, the growth outermost surface is formed to extend in a direction perpendicular to the crystal growth direction), the (0001) facet 5
  • the condition is to make the end of the ingot 10 a minimum.
  • the temperature of each point such as the central portion 14, the end portion 15, and the outermost circumference portion 16 in the growth outermost surface of the ingot 10 shown in FIG. 7 is important.
  • the end 15 is located at an end area of the ingot 10 and at a distance within 10% of the diameter of the ingot 10 from the inner wall of the crucible 11.
  • the relationship satisfies the relational expression Tc> Tb ⁇ ⁇ ⁇ ⁇ Ta, and the temperatures Tb and Ta It is preferable that the temperature gradient ((absolute value of difference between temperature Ta and temperature Tb) / (distance between central portion 14 and end 15)) satisfies a relationship of 10 ° C./cm or less.
  • the height of the ingot 10 (the distance from the surface of the base substrate 1 to the surface of the ingot 10) is measured at a pitch of 5 mm between the central portion 14 and the end portion 15. Then, the radius of the arc corresponding to the surface of the ingot 10 between the pitches is calculated from the difference in height between the pitches. Then, the minimum radius of the radii of the arc calculated for each pitch between the central portion 14 and the end portion 15 is taken as the above-mentioned radius of curvature.
  • the flatness of the surface of the ingot 10 may be measured by the following measurement method. That is, the height of the surface of the ingot 10 from the reference plane is measured at a plurality of positions (measurement points) arranged in a cross direction (preferably, 5 mm pitch matrix) with a 5 mm pitch from the center of the surface of the ingot 10 Do. Then, the difference in height is measured between adjacent measurement points. Further, an angle corresponding to the inclination of the surface of the ingot 10 between the adjacent measurement points is determined from the tangent (tan) which can be determined from the difference in height and the distance between the measurement points. It is preferable that the average of the angle is 10 degrees or less about the several angle calculated
  • the absolute value of the difference between the temperature Tb and the temperature Tc is 1 ° C. or more and 50 ° C. or less (more specifically, the temperature Tc is more than the temperature Tb It is preferable that the temperature is high and the difference between the temperature Tb and the temperature Tc is 1 ° C. or more and 50 ° C. or less).
  • the absolute value of the difference is less than 1 ° C., polycrystals of silicon carbide easily adhere and grow on the inner peripheral surface of the crucible 11 made of graphite, and as a result, the growth of the single crystal ingot is hindered. become.
  • the temperature of the end surface part of the ingot 10 also rises under the influence of the radiant heat etc. from the crucible 11 side. As a result, the temperature difference between the central portion 14 and the end portion 15 becomes large, and the flatness of the surface of the ingot 10 can not be maintained.
  • the width of the (0001) facet 5 (the width of the base substrate 1 in the off direction) is preferably 10% or less of the diameter of the ingot 10.
  • the side surface of the crucible 11 is heated, so that the temperature distribution tends to occur in the radial direction of the ingot 10 in the temperature raising step. Therefore, if the time until the bottom surface temperature of the crucible 11 reaches 2000 ° C. or more is 1 hour or less, the temperature distribution is maintained for 5 minutes or more at the expected growth temperature under an atmospheric pressure of 40 kPa or more and 100 kPa or less. After homogenization, it is preferable to reduce the atmospheric pressure to the growth expected pressure.
  • the ingot 10 grows to a height of 1 cm or more, so the temperature of the outermost surface of the growth rises from the initial stage of the growth. As a result, the temperature gradient between the growth outermost surface of the ingot 10 and the raw material decreases. Therefore, it is considered that the temperature environment at the end portion 15 and the outermost portion 16 changes from the initial state of growth, and in some cases, the magnitude relationship between the temperature Tb of the end portion 15 and the temperature Tc of the outermost portion 16 is reversed. Be In such a state, the shape of the ingot 10 becomes concave, and the (0001) facet 5 moves from the end of the ingot 10 to the center.
  • the temperature of Tc> the temperature Tb is always maintained by raising the side temperature of the crucible 11 from the initial stage of growth or by increasing the heat release from the upper side of the crucible 11
  • the surface shape of the ingot 10 be a flat shape and a slightly convex shape.
  • the outermost surface of the raw material for forming the ingot 10 be flat in advance so that the loading depth of the raw material does not vary.
  • the size of the (0001) facet 5 is also small, and the flatness of the surface of the ingot 10 is high. Therefore, the dislocation occurrence probability is substantially uniform over the entire surface of the ingot 10, and decreases uniformly as the ingot 10 grows. That is, in the ingot 10 according to the present invention, dislocations can be reduced substantially throughout the region.
  • the temperature of the part generating the facets is higher than the temperature of the other parts. That is, the relationship between the temperature Td of the facet side end 17 and the temperature Te of the facet side outermost periphery 18 in FIG. 7 is Te> Td, and the temperature difference between the facet side end 17 and the facet side outermost periphery 18 ( That is, it is preferable to set Te-Td) to 20 ° C. or more and 100 ° C. or less. In addition, if the temperature difference between the central portion 14 and the end portion 15 is large, the facet region widens, so the temperature gradient between the central portion 14 and the end portion 15 should be 20 ° C./cm or less. preferable.
  • a relatively large temperature difference is formed only between the facet side end 17 and the facet side outermost periphery 18, and in the other part of the outer periphery of the ingot 10, the end 15 and the outermost periphery 16
  • the temperature difference between them is 20.degree. C. or less. In order to do this, for example, it is possible to heat only the place where the facet 5 is to be formed.
  • the center line of crucible 11 is specified on the side which forms (0001) facet 5
  • the thickness of the heat insulating material around the crucible 11 is thicker than the other areas only in the area where the facets 5 are formed (for example, about 2 mm to 10 cm less than the thickness of the heat insulating material in other parts Thick).
  • the hole (heat dissipation hole) formed for heat dissipation is closed in the region opposite to the portion where the facet 5 is formed in the upper part of the crucible 11.
  • the temperature control member 3 is disposed inside the support member 2 and the heating temperature of the region (end of the base substrate 1) where the facet 5 is desired to be formed is
  • the position of the facet 5 may be placed at the end of the ingot 10 by a method of comparison (for example, higher than the temperature of the other part).
  • a temperature control member 3 for example, a heating member such as an electric heater can be used.
  • a source gas for growing silicon carbide on base substrate 1 is intensively supplied to the region where facet 5 is to be formed. Or adjust the arrangement of the discharge part when discharging the source gas used for growing silicon carbide from the inside of the processing vessel, and the growth rate of silicon carbide in the area where the facet 5 is to be formed You may use the method of raising more.
  • the post-processing step (S30) is performed. Specifically, the formed ingot 10 is taken out from the inside of the processing vessel, and the surface layer is ground, a mark indicating the crystal orientation of the ingot 10 is formed in the ingot 10, and the base substrate 1 is separated from the ingot 10 And perform necessary post-processing.
  • the maximum radius of curvature in the cross section shown in FIG. 5 is the planar shape of ingot 10 shown in FIG.
  • the radius of the circumscribed circle (when the planar shape is a circular ingot 10 as shown in FIG. 4, the circle that forms the outer periphery of the planar shape of the ingot 10) is preferably at least three times the radius.
  • the high concentration nitrogen region 6 is disposed on the upstream side in the off-angle direction indicated by the arrow 26.
  • the off-angle direction is a direction in which the off-angle in the base substrate 1 is set, and is, for example, either a ⁇ 11-20> direction or a ⁇ 1-100> direction.
  • the nitrogen concentration in the high concentration nitrogen region 6 is 1.1 times or more that of the nitrogen region of the low concentration nitrogen region 7. The nitrogen concentration can be evaluated, for example, by SIMS.
  • the light transmittance per unit thickness in the high concentration nitrogen region 6 is the unit thickness in the low concentration nitrogen region 7 which is a portion other than the high concentration nitrogen region 6 of the ingot 10. It is lower than the light transmittance of the above.
  • the transmittance of the light can be measured, for example, using FTIR (Fourier transform infrared spectrometer).
  • the thickness of the substrate 20 is 400 ⁇ m, and the transmittance of light of the above wavelength in the thickness direction of the substrate 20 in the high concentration nitrogen region 6 of the substrate 20 and the thickness of the substrate 20 in the low concentration nitrogen region 7 of the substrate 20 A method may be used in which the transmittance of light of the above wavelength in the longitudinal direction is measured using a visible light spectrometer.
  • the high concentration nitrogen region 6 having a relatively high nitrogen concentration is disposed at the end of the ingot 10
  • the low concentration nitrogen region 7 having a relatively low nitrogen concentration is , And can be formed as a united area including the central portion of the ingot 10. Therefore, when cutting silicon carbide substrate 20 from ingot 10, silicon carbide substrate 20 can be easily obtained in which relatively low concentration nitrogen region 7 is formed in a wide region including the central portion of the substrate.
  • a silicon carbide substrate 20 shown in FIG. 6 is manufactured using the process shown in FIG. A method of manufacturing silicon carbide substrate 20 will be specifically described with reference to FIG.
  • an ingot preparing step (S40) is performed.
  • the ingot 10 which consists of silicon carbides obtained by implementing the process shown in FIG. 1 is prepared.
  • the slicing step (S50) is performed. Specifically, in the step (S50), the ingot 10 is sliced by any method.
  • a method of slicing for example, a method using a wire saw or a method using a cutting member (for example, an inner peripheral blade) on which hard abrasive grains such as diamond are disposed on the surface can be used.
  • a direction for slicing ingot 10 for example, ingot 10 may be sliced in a direction along surface 4 of base substrate 1 (direction along straight line 8 shown in FIG. 5).
  • the high concentration nitrogen region 6 can be disposed at the end of the silicon carbide substrate 20.
  • the ingot 10 may be sliced.
  • the post-processing step (S60) is performed. Specifically, the mirror surface is finished to an arbitrary surface state by grinding and polishing the front surface and / or the back surface of the sliced substrate. Thus, a silicon carbide substrate 20 as shown in FIG. 6 is obtained. In silicon carbide substrate 20, most of the main surface including the central portion is low concentration nitrogen region 7, and high concentration nitrogen region 6 is disposed at the end. Further, as shown in FIG. 8, recess 21 may be formed on the outer periphery of silicon carbide substrate 20 by removing high concentration nitrogen region 6 by grinding or the like. In this case, almost the entire surface of silicon carbide substrate 20 is low concentration nitrogen region 7, and silicon carbide substrate 20 having uniform characteristics can be obtained.
  • a silicon carbide epitaxial layer excellent in uniformity of characteristics can be easily formed on the surface of the silicon carbide substrate 20.
  • the method for manufacturing the silicon carbide substrate shown in FIG. 8 it is possible to obtain a silicon carbide substrate 20 having no high concentration nitrogen region, that is, the entire surface is a low concentration nitrogen region.
  • the silicon carbide substrate 20 shown in FIG. 8 basically has the same configuration as the silicon carbide substrate 20 shown in FIG. 6, but the high concentration nitrogen region 6 shown in FIG. 6 is removed. Therefore, in silicon carbide substrate 20 shown in FIG. 8, recess 21 is formed in a part of the outer peripheral end portion which is a region where high concentration nitrogen region 6 was located.
  • recess 21 is located at the end of silicon carbide substrate 20 in the off-angle direction.
  • a substrate having a circular planar shape is used as base substrate 1, but a substrate of any other shape can be used as base substrate 1.
  • a substrate having a rectangular planar shape is used as the base substrate 1
  • an ingot 10 having a substantially rectangular planar shape can be obtained as shown in FIG.
  • the facet 5 can be disposed at the end when the ingot 10 is viewed in plan.
  • the cross section taken along line VV of FIG. 9 is the same as the cross section shown in FIG.
  • the maximum radius of curvature (maximum radius of curvature of the outermost surface 9 of FIG. 5) at the outermost surface of the obtained ingot 10 is at least three times the radius of the circumscribed circle 25 of the planar shape of the ingot 10 shown in FIG. Is preferred.
  • silicon carbide substrate 20 having a planar shape as shown in FIG. 10 is obtained by slicing ingot 10 along a direction parallel to surface 4 of base substrate 1 (that is, a direction shown by straight line 8 in FIG. 5). You can get Also in silicon carbide substrate 20 shown in FIG. 10, high concentration nitrogen region 6 is arranged at the end, and the other region is low concentration nitrogen region 7. With such a silicon carbide substrate 20, the same effect as that of the silicon carbide substrate 20 shown in FIG. 6 can be obtained.
  • the silicon carbide substrate 20 shown in FIG. 10 by grinding or the like, the silicon carbide substrate 20 whose entire surface has become the low concentration nitrogen region 7 as shown in FIG. It can also be done.
  • the high concentration nitrogen region 6 may be previously removed from the ingot 10 in the step of forming the ingot 10 (specifically, the post-processing step (S30) shown in FIG. 1). With such a silicon carbide substrate 20, the same effect as the silicon carbide substrate 20 shown in FIG. 8 can be obtained.
  • base substrate 1 for forming ingot 10 a substrate having a rectangular planar shape as shown in FIG. 12 and made of silicon carbide single crystal can also be used.
  • the ingot 10 having a planar shape as shown in FIG. 12 can be formed using the ingot manufacturing method shown in FIG.
  • the cross-sectional shape of the ingot 10 along the line VV shown in FIG. 12 is basically the same as the cross-sectional shape of the ingot 10 shown in FIG.
  • the maximum radius of curvature of the outermost surface 9 is preferably at least three times the radius of the circumscribed circle 25 of the planar shape of the ingot 10 shown in FIG. .
  • the ingot 10 shown in FIG. 12 is sliced and post-processed by the method shown in FIG. 2 to obtain a silicon carbide substrate 20 having a rectangular planar shape as shown in FIG.
  • the slice direction is a direction parallel to the paper surface of FIG. 12 (a direction along the surface of the base substrate).
  • the high concentration nitrogen region 6 is formed at the end, while the other most region is the low concentration nitrogen region 7.
  • silicon carbide substrate 20 whose entire surface is low concentration nitrogen region 7 is obtained as shown in FIG. it can.
  • the high concentration nitrogen region 6 may be removed from the ingot 10, and then the ingot 10 may be sliced to obtain the silicon carbide substrate 20 shown in FIG. .
  • a substrate having a hexagonal planar shape can also be used as the base substrate 1.
  • an ingot 10 having a hexagonal planar shape can be obtained as shown in FIG.
  • the (0001) facet 5 can be disposed at the end of the outermost surface 9 (see FIG. 5) of the crystal growth portion of the ingot 10.
  • the sectional view taken along line VV of the ingot 10 shown in FIG. 15 is the same as the sectional view shown in FIG.
  • the maximum radius of curvature (maximum radius of curvature of the outermost surface 9 of FIG. 5) in the outermost surface 9 of the obtained ingot 10 is at least three times the radius of the circumscribed circle 25 of the planar shape of the ingot 10 shown in FIG. It is preferable that
  • the silicon carbide substrate 20 having a hexagonal planar shape as shown in FIG.
  • the slice direction is a direction parallel to the paper surface of FIG. 15 (a direction along the surface of the base substrate 1).
  • the high concentration nitrogen region 6 is disposed at the end, while the remaining region is the low concentration nitrogen region 7. Also in this case, the same effect as the substrate shown in FIG. 6 can be obtained.
  • a silicon carbide substrate whose entire surface has become a low concentration nitrogen region 7 as shown in FIG. 17 by removing high concentration nitrogen region 6 from silicon carbide substrate 20 shown in FIG. 16 using grinding or the like. You can also get twenty.
  • the high concentration nitrogen region 6 may be removed from the ingot 10 at the stage when the ingot 10 shown in FIG. 15 is formed, and then the ingot 10 may be sliced to obtain the silicon carbide substrate 20 shown in FIG. .
  • the method of manufacturing silicon carbide ingot 10 according to the present invention is, as shown in FIG. 1, in the off angle direction which is either the ⁇ 11-20> direction or the ⁇ 1-100> direction with respect to the (0001) plane.
  • Preparing a base substrate 1 having an off angle of 0.1 ° to 10 °, more preferably 1 ° to 10 ° and made of single crystal silicon carbide (preparation step (S10)); And a step of growing a silicon carbide layer on the surface (film forming step (S20)).
  • the film forming step (S20) when considering the intersection angle at which the ⁇ 0001> direction axis of the base substrate 1 intersects the surface 4 of the base substrate 1 in the off angle direction, the intersection angle is the acute side.
  • a region having (0001) facet 5 is formed on the surface of the grown silicon carbide layer.
  • a region with a relatively high nitrogen concentration (high concentration nitrogen located under the (0001) facet) Region 6) can be arranged at the end of silicon carbide ingot 10. Therefore, a region having a relatively low nitrogen concentration (a low concentration nitrogen region 7 which is a region other than the high concentration nitrogen region) can be formed as a region including the central portion of silicon carbide ingot 10. Therefore, when cutting out silicon carbide substrate 20 from ingot 10, it is possible to easily obtain silicon carbide substrate 20 having low concentration nitrogen region 7 formed in a wide region including the central portion of the substrate.
  • the low concentration nitrogen region 7 that is, a region having a stable nitrogen concentration without much incorporation of nitrogen
  • a semiconductor element is formed on the surface of silicon carbide substrate 20 In this case, the utilization efficiency of the substrate can be increased to efficiently form a semiconductor element.
  • the portion located below the region having the (0001) facet is the silicon carbide layer
  • the high concentration nitrogen region 6 may have a nitrogen concentration higher than that of the portion (low concentration nitrogen region 7) other than the portion located below the region having the facet surface.
  • the high concentration nitrogen region 6 is formed below the region having the (0001) facet 5, and the portion including the central portion of the other ingot becomes the low concentration nitrogen region 7 having a lower nitrogen concentration than the high concentration nitrogen region 6. Therefore, by slicing the silicon carbide ingot 10, the silicon carbide substrate 20 in which the wide region including the central portion of the surface is the low concentration nitrogen region 7 can be easily obtained.
  • the width of the high concentration nitrogen region 6 in the off-angle direction is 1/10 or less of the width of the base substrate 1 in the off-angle direction. It may be.
  • the size of high concentration nitrogen region 6 is sufficiently smaller than the whole of silicon carbide ingot 10, high concentration nitrogen region 6 is formed on the surface (main surface) of silicon carbide substrate 20 obtained from silicon carbide ingot 10.
  • the occupied area can be reduced.
  • the width of the low concentration nitrogen region 7 (stabilized with nitrogen concentration) on the surface of silicon carbide substrate 20 can be made sufficiently wide.
  • high concentration nitrogen region 6 can be easily removed in the outer peripheral grinding and forming step of silicon carbide ingot 10, it is possible to suppress an increase in the time required for processing silicon carbide ingot 10 concerned.
  • the method for producing a silicon carbide ingot may further include the step of removing the high concentration nitrogen region (post-processing step (S30) in FIG. 1).
  • most of silicon carbide ingot 10 can be constituted by low concentration nitrogen region 7. Therefore, the surface of silicon carbide substrate 20 cut out from silicon carbide ingot 10 can be formed of only low concentration nitrogen region 7, so that silicon carbide substrate 20 with stable nitrogen concentration and excellent homogeneity can be obtained.
  • the transmittance of light having a wavelength of 450 nm to 500 nm per unit thickness in the high concentration nitrogen region 6 is a silicon carbide layer (silicon carbide layer grown on the base substrate 1)
  • the light transmittance per unit thickness in a portion (low concentration nitrogen region 7) other than the high concentration nitrogen region may be lower than the light transmittance.
  • the light transmittance of the silicon carbide ingot 10 tends to decrease as the nitrogen concentration increases. Therefore, the characteristics of the light transmittance also differ between the high concentration nitrogen region 6 and the region other than the high concentration nitrogen region (low concentration nitrogen region 7). Therefore, according to the present invention, since the region (the high concentration nitrogen region 6) in which the light transmittance is relatively low is disposed at the end of the silicon carbide ingot 10, the light transmittance With regard to the characteristics described above, the region (low concentration nitrogen region 7) in which the light transmittance is relatively high can be formed as a region including the central portion of the silicon carbide ingot 10. Therefore, when silicon carbide substrate 20 is cut out from silicon carbide ingot 10, silicon carbide substrate 20 in which the region having a relatively high light transmittance is formed in a wide region including the central portion of the substrate is easily obtained. Can.
  • the micropipe density of the portion (high concentration nitrogen region 6) located below the region having the (0001) facet is lower than the region having the (0001) facet in the silicon carbide layer. It may be higher than the micropipe density in the portion (low concentration nitrogen region 7) other than the above-mentioned portion located.
  • the region (low concentration nitrogen region 7) can be formed as a region including the central portion of silicon carbide ingot 10. Therefore, when cutting silicon carbide substrate 20 from silicon carbide ingot 10, a silicon carbide substrate in which a region (low concentration nitrogen region 7) having a relatively low micropipe density is formed in a wide region including the central portion of the substrate. 20 can be easily obtained.
  • the maximum radius of curvature of the surface (the outermost surface 9 shown in FIG. 5) of the silicon carbide layer after the step of growing the silicon carbide layer (film forming step (S20)) is the base It may be three or more times the radius of the circumscribed circle 25 with respect to the planar shape of the substrate 1. Further, the maximum radius of curvature of the surface (uppermost surface 9 in FIG. 5) of the silicon carbide layer is the maximum radius of curvature in the region (uppermost surface) including the portion farthest from the surface of base substrate 1 in the silicon carbide layer. Is preferred.
  • the volume of the silicon carbide layer formed on base substrate 1 can be made sufficiently large, and as a result, the volume of silicon carbide ingot 10 can be made sufficiently large. Therefore, when cutting silicon carbide substrate 20 from silicon carbide ingot 10, silicon carbide substrate 20 with a large area can be obtained efficiently.
  • the planar shape of the silicon carbide layer (the silicon carbide epitaxial growth layer formed of the high concentration nitrogen region 6 and the low concentration nitrogen region 7) is larger than that of the base substrate 1 (for example, away from the base substrate 1)
  • the silicon carbide layer may be formed in such a manner that the planar shape becomes larger in accordance with the above, or that the side wall is inclined toward the outside as being away from the base substrate 1.
  • Silicon carbide ingot 10 according to the present invention is manufactured using the method for manufacturing silicon carbide ingot 10 described above.
  • the region having a relatively low nitrogen concentration (low concentration nitrogen region 7) can be formed as a region including the central portion of silicon carbide ingot 10. Therefore, by cutting silicon carbide substrate 20 out of silicon carbide ingot 10, silicon carbide substrate 20 in which low concentration nitrogen region 7 having a relatively low nitrogen concentration is formed in a wide region including the central portion of the substrate can be easily obtained. Can.
  • a step of preparing a silicon carbide ingot using the method of manufacturing silicon carbide ingot 10 (ingot preparing step (S40)); And a step of slicing the silicon carbide ingot 10 (a slicing step (S50)).
  • silicon carbide ingot 10 a region having a relatively low nitrogen concentration (low concentration nitrogen region 7 which is a region other than the high concentration nitrogen region) is formed as a region including the central portion of silicon carbide ingot 10 Be done. Therefore, carbonization is performed by cutting out silicon carbide substrate 20 from silicon carbide ingot 10 in the slicing step (S50) to form low concentration nitrogen region 7 having a relatively low nitrogen concentration in a wide region including the central portion of the substrate.
  • the silicon substrate 20 can be easily obtained.
  • the step of preparing a silicon carbide ingot in the step of preparing a silicon carbide ingot (ingot preparing step (S40)), in the silicon carbide layer after the step of growing a silicon carbide layer (film forming step (S20)), )
  • the portion located under the region having facets is higher in nitrogen concentration than the portion (the low concentration nitrogen region 7) other than the portion located under the region having (0001) facets in the silicon carbide layer It may be a concentration nitrogen region 6.
  • the step of removing the high concentration nitrogen region 6 from the silicon carbide ingot 10 before the slicing step (S50) of slicing the silicon carbide ingot 10 for example, the post treatment step (S30 in FIG. 1)
  • the method of manufacturing silicon carbide substrate 20 is a step of preparing silicon carbide ingot using the method of manufacturing silicon carbide ingot 10 as shown in FIG.
  • the step of preparing the silicon carbide ingot including the preparing step (S40) (ingot preparing step (S40)), in the silicon carbide layer after the step of growing the silicon carbide layer (film forming step (S20)), )
  • the portion located under the region having facets is higher in nitrogen concentration than the portion (the low concentration nitrogen region 7) other than the portion located under the region having (0001) facets in the silicon carbide layer
  • the step of removing the high concentration nitrogen region 6 from the silicon carbide ingot 10 for example, the post-treatment step of FIG. 30) a step of grinding and removing the high concentration nitrogen region 6 contained in 30) and a step of removing the high concentration nitrogen region 6 and then slicing the silicon carbide ingot 10 (slice step (S50))
  • the step of preparing the silicon carbide ingot including the preparing step (S
  • Silicon carbide substrate 20 according to the present invention is manufactured using the above-described method for manufacturing a silicon carbide substrate. In this way, silicon carbide substrate 20 can be easily realized in which low concentration nitrogen region 7 having a relatively low nitrogen concentration is formed in a wide region including the central portion of the substrate.
  • the method for manufacturing a silicon carbide ingot according to the present invention includes an off angle direction (direction indicated by arrow 26 in FIG. 3) which is either the ⁇ 11-20> direction or the ⁇ 1-100> direction with respect to the (0001) plane. And a step of preparing the base substrate 1 made of single crystal silicon carbide (preparing step (S10)), and the base substrate. Forming a silicon carbide layer on the surface of the silicon substrate 1 (film forming step (S20)), and in the film forming step (S20), the ⁇ 0001> direction axis of the base substrate 1 is the base substrate 1 in the off angle direction.
  • a region having (0001) facet 5 is formed on the surface of the grown silicon carbide layer at the upstream end where the intersection angle is an acute angle when considering the intersection angle intersecting with surface 4 The .
  • the portion located under the region having (0001) facet 5 (high concentration nitrogen region 6) is below the region having (0001) facet 5 in the silicon carbide layer.
  • the transmittance per unit thickness of light having a wavelength of 450 nm or more and 500 nm or less is lower than that of the portion (low concentration nitrogen region 7) other than the portion located in.
  • the nitrogen taken in from the (0001) facet 5 during the growth of the silicon carbide layer can be obtained. Since the region (high concentration nitrogen region 6) where the light transmittance is reduced due to it is arranged at the end of silicon carbide ingot 10 (the part under (0001) facet 5), the center of silicon carbide ingot 10 The other portion including the portion (the low concentration nitrogen region 7) can be a region having a relatively high light transmittance. Therefore, when cutting out silicon carbide substrate 20 from silicon carbide ingot 10, carbonization is performed in a wide region including the central portion of the region (low concentration nitrogen region 7) in which the light transmittance is relatively high.
  • the silicon substrate 20 can be easily obtained. As described above, a relatively high light transmittance region (a region with stable nitrogen concentration and transmittance with little incorporation of nitrogen) can be formed in a wide region including the central portion of the substrate, so that the semiconductor element is formed on the substrate surface. In forming the semiconductor device, the semiconductor element can be efficiently formed.
  • Silicon carbide ingot 10 has an off angle of at least 0.1 ° to 10 ° in the off-angle direction, which is either the ⁇ 11-20> direction or the ⁇ 1-100> direction with respect to the (0001) plane.
  • a base substrate 1 made of single crystal silicon carbide and a silicon carbide layer formed on the surface of the base substrate 1 are provided below, more preferably at 1 ° to 10 °.
  • the grown carbonized at the upstream end that is the side where the crossing angle becomes an acute angle A region having a (0001) facet 5 is formed on the surface of the silicon layer.
  • the portion located below the region having the (0001) facet 5 is a portion other than the above portion located below the region having the (0001) facet in the silicon carbide layer It may be a high concentration nitrogen region 6 in which the nitrogen concentration is higher than the low concentration nitrogen region 7).
  • the nitrogen concentration of the high concentration nitrogen region 6 is 1.1 times or more the nitrogen concentration in the portion (low concentration nitrogen region 7) other than the portion located below the region having the (0001) facet 5 It may be
  • the high concentration nitrogen region 6 and the low concentration nitrogen region 7 can be easily distinguished by the nitrogen concentration, the light transmittance, and the like. Therefore, when the high concentration nitrogen region 6 is removed from the silicon carbide ingot 10 by grinding or the silicon carbide substrate 20 is cut out from the silicon carbide ingot 10 and a device is formed on the surface of the silicon carbide substrate 20, the high concentration nitrogen It is possible to easily perform an operation of forming a device so as to avoid the region 6 (or not to straddle the boundary between the high concentration nitrogen region 6 and the low concentration nitrogen region 7).
  • the width of the high concentration nitrogen region 6 in the off angle direction may be 1/10 or less of the width of the base substrate 1 in the off angle direction. In this case, since the size of the high concentration nitrogen region 6 is reduced, the size of the region other than the high concentration nitrogen region 6 (low concentration nitrogen region 7) can be secured sufficiently large.
  • the transmittance of light having a wavelength of 450 nm to 500 nm per unit thickness in the high concentration nitrogen region 6 is a portion (low concentration nitrogen region 7) other than the high concentration nitrogen region in the silicon carbide layer. It may be lower than the light transmittance per unit thickness in the above.
  • the high concentration nitrogen region 6 and the low concentration nitrogen region 7 can be easily distinguished by the light transmittance. Therefore, an operation such as removal of high concentration nitrogen region 6 by grinding from silicon carbide ingot 10 can be easily performed.
  • the transmittance in the high concentration nitrogen region 6 may be 5% or more lower than the transmittance in the low concentration nitrogen region 7, which is a portion other than the high concentration nitrogen region in the silicon carbide layer. .
  • the high concentration nitrogen region 6 and the low concentration nitrogen region 7 can be easily distinguished from the difference in transmittance.
  • the micropipe density of the portion (high concentration nitrogen region 6) located below the region having the (0001) facet surface is located below the region having the (0001) facet surface 5 in the silicon carbide layer. It may be higher than the micropipe density in the part other than the part (the low concentration nitrogen region 7).
  • a portion other than the portion located below the region having (0001) facet 5 (low-concentration nitrogen region 7 having a relatively low micropipe density) includes the central portion of silicon carbide ingot 10. Formed as a Therefore, when cutting silicon carbide substrate 20 from ingot 10, silicon carbide substrate 20 can be easily obtained in which the region with a relatively low micropipe density is formed in a wide region including the central portion of the substrate.
  • the micropipe density of the portion (high concentration nitrogen region 6) located under the region having (0001) facet 5 is located under the region having (0001) facet 5 in the silicon carbide layer.
  • the density may be 1.2 times or more the micropipe density in the portion other than the portion concerned (the low concentration nitrogen region 7).
  • the micropipe density is relatively low as a result, and therefore the central portion is included.
  • a silicon carbide ingot 10 can be obtained in which the micropipe density is reduced for the region.
  • the maximum radius of curvature of the surface (the outermost surface 9 shown in FIG. 5) of the silicon carbide layer may be three or more times the radius of the circumscribed circle 25 related to the planar shape of the base substrate 1.
  • the volume of the silicon carbide layer formed on base substrate 1 can be made sufficiently large, and as a result, the volume of silicon carbide ingot 10 can be made sufficiently large.
  • Silicon carbide substrate 20 according to the present invention is obtained by slicing silicon carbide ingot 10 described above. In this way, it is possible to easily obtain silicon carbide substrate 20 in which low concentration nitrogen region 7 (or a region with high light transmittance) having a relatively low nitrogen concentration is formed in a wide region including the central portion of the substrate. it can.
  • the silicon carbide substrate 20 according to the present invention may be obtained by slicing the silicon carbide ingot 10 after removing the high concentration nitrogen region 6 from the silicon carbide ingot 10 described above. In this way, the high concentration nitrogen region 6 (the region with low light transmittance) is removed in advance, so that the low concentration nitrogen region 7 (with high light transmittance) has a lower nitrogen concentration than the high concentration nitrogen region 6.
  • the silicon carbide substrate 20 is formed using the silicon carbide ingot 10 in which the region (the region higher than the concentration nitrogen region) is a major part (or constituted only by the low concentration nitrogen region 7). Therefore, it is possible to obtain silicon carbide substrate 20 in which fluctuations in nitrogen concentration and light transmittance are reduced.
  • the variation of the nitrogen concentration relative to the average value may be 10% or less. In this case, since the variation in nitrogen concentration is sufficiently small so as not to adversely affect the characteristics of silicon carbide substrate 20, silicon carbide substrate 20 having uniform characteristics can be reliably obtained.
  • the variation of the dislocation density with respect to the average value may be 80% or less. Also, the variation with respect to the average value of dislocation density in the low concentration nitrogen region 7 may be 80% or less. In this case, if variations in dislocation density as described above occur, changes in characteristics in the main surface of silicon carbide substrate 20 can be suppressed to a practically acceptable level.
  • the nitrogen concentration is relatively higher at one end in either the ⁇ 11-20> direction or the ⁇ 1-100> direction than the other part.
  • a high concentration nitrogen region 6 is formed.
  • the ⁇ 0001> direction axis of silicon carbide substrate 20 is the same as that of silicon carbide substrate 20 in either the ⁇ 11-20> direction or the ⁇ 1-100> direction (off angle direction).
  • the crossing angle which intersects to the surface it may be formed at the end on the upstream side which is the side where the crossing angle becomes an acute angle. In this way, when growing silicon carbide ingot 10 used to form silicon carbide substrate 20, silicon carbide substrate with high concentration nitrogen region 6 can be easily controlled by controlling the arrangement of (0001) facet 5 It can be placed at the end of 20.
  • the size (for example, the maximum width in plan view) of silicon carbide substrate 20 may be 4 inches or more. If the present invention is applied to a silicon carbide substrate 20 having a size of 4 inches or more, remarkable effects can be obtained particularly in terms of the device manufacturing efficiency.
  • the nitrogen concentration of the high concentration nitrogen region 6 may be 1.1 times or more the nitrogen concentration in the other portion.
  • the high concentration nitrogen region 6 and the other part (low concentration nitrogen region 7) other than the high concentration nitrogen region can be easily distinguished by the light transmittance or the like.
  • the width of the high concentration nitrogen region 6 in either the ⁇ 11-20> direction or the ⁇ 1-100> direction is 1/10 of the width in the above direction of the silicon carbide substrate 20. It may be the following. In this case, since the size of the high concentration nitrogen region 6 is reduced, the size of the region other than the high concentration nitrogen region 6 (low concentration nitrogen region 7) can be secured sufficiently large.
  • the transmittance of light having a wavelength of 450 nm to 500 nm per unit thickness in the high concentration nitrogen region 6 is in a portion (low concentration nitrogen region 7) other than the high concentration nitrogen region. It may be lower than the transmittance of light having a wavelength of 450 nm or more and 500 nm or less per unit thickness.
  • the transmittance in the high concentration nitrogen region 6 may be 5% or more lower than the transmittance in a portion other than the high concentration nitrogen region (low concentration nitrogen region 7).
  • the high concentration nitrogen region 6 and the low concentration nitrogen region 7 can be easily distinguished by the light transmittance. Therefore, when the device is formed on the surface of the silicon carbide substrate 20, the device is avoided so as to avoid the high concentration nitrogen region 6 (or so as not to cross the boundary portion between the high concentration nitrogen region 6 and other regions). Can be easily performed.
  • the micropipe density of the high concentration nitrogen region 6 may be higher than the micropipe density in a portion other than the high concentration nitrogen region (low concentration nitrogen region 7). Furthermore, in the silicon carbide substrate 20, the micropipe density of the high concentration nitrogen region 6 may be 1.2 or more times the micropipe density in a portion (low concentration nitrogen region 7) other than the high concentration nitrogen region.
  • the micropipe density is reduced for low concentration nitrogen region 7, which is a region that occupies most of the silicon carbide substrate, when forming a silicon carbide epitaxial layer on the surface of silicon carbide substrate 20, It is possible to suppress the generation of defects caused by the micropipe on the silicon carbide substrate 20 side in the silicon carbide epitaxial layer.
  • the variation of the nitrogen concentration relative to the average value may be 10% or less.
  • the variation in nitrogen concentration is sufficiently small so as not to adversely affect the characteristics of the silicon carbide substrate, it is possible to reliably obtain a silicon carbide substrate having uniform characteristics.
  • the variation with respect to the average value of dislocation density may be 80% or less. Further, the variation with respect to the average value of dislocation density in the low concentration nitrogen region may be 80% or less. In this case, the variation in the dislocation density as described above can suppress the change in the characteristics in the main surface of the silicon carbide substrate to a practically acceptable level.
  • facets can be brought close to the end in the silicon carbide ingot 10.
  • the substrate 20 without the entire facet.
  • the nitrogen doping amount and the main dislocation are different between the facet and the region other than the facet.
  • the nitrogen doping amount of the silicon carbide substrate affects the CMP polishing rate. Therefore, the nitrogen doping amount of the substrate 20 is preferably uniform.
  • the substrate size is 4 inches or more, the warpage of the substrate 20 and the TTV also increase accompanying the increase in the substrate size.
  • the influence of the nitrogen doping amount is also remarkable. That is, when the variation in the amount of nitrogen doping on the substrate surface also decreases, the variation in internal stress distribution due to impurities such as nitrogen decreases, and the warpage and TTV also improve.
  • the above-described nitrogen doping amount and the like also affect the process of forming the device (for example, the heat treatment process). That is, since the absorptivity of light in the substrate changes when the nitrogen doping amount is different, a local temperature difference occurs when the substrate is heated.
  • the size of the substrate 20 is small, the effect of the temperature difference is not large due to the effect of heat conduction, but when the size of the substrate becomes 4 inches or more, the heat conduction effect becomes smaller as the temperature becomes higher, Temperature distribution on the substrate 20 is likely to occur.
  • temperature conditions vary in the plane of the substrate, which causes a problem that uniform film can not be formed on the surface of the substrate.
  • the nitrogen doping amount uniformity Is high so that the occurrence of the above problems can be suppressed.
  • the nitrogen doping amount (nitrogen concentration) described above can be measured by SIMS.
  • the nitrogen concentration in the portion where the nitrogen doping amount is high is 1.5 times or more the nitrogen concentration in the other region.
  • the transmittance of light having a wavelength of 400 nm or more and 500 nm or less preferably satisfies the following conditions when the thickness of the substrate 20 is 400 ⁇ m. That is, when the transmittance of the light is measured at a plurality of locations (for example, 10 locations including the central portion) of the substrate 20 using a visible light spectrometer, the average transmittance is preferably 20% to 65%. . In addition, for most of the main surface (area of 70% or more in area ratio) of the main surface of the substrate, local transmittance is within ⁇ 20% of the average transmittance with respect to the average transmittance. preferable.
  • the refractive index of the substrate 20 is preferably 2.5 or more and 2.8 or less.
  • the dislocation was treated by visualizing and measuring the surface of the substrate by etching using molten salt KOH as an etching solution. Specifically, the molten salt KOH is heated to 500 ° C., and the substrate 20 is immersed in the molten molten KOH solution for about 1 to 10 minutes. As a result, pits are formed on the surface of the substrate 20 corresponding to the presence of dislocations. Then, the number of the pits was counted with a Nomarski differential interference microscope and divided by the area of the measurement range to calculate the number of pits per unit area (that is, the number of dislocations per unit area).
  • dislocation density micropipe density of the base substrate 1 10 ⁇ 100cm -2
  • etch pit density EPD: When 1 ⁇ 5E4cm -2, from the base substrate 1 in the ingot 10 in accordance with the present invention
  • the micropipe density and the etch pit density are reduced to about 1/2 to 1/20 of the base substrate 1.
  • sample The silicon carbide ingot and the silicon carbide ingot were sliced as follows, and the sample of the Example of this invention and the comparative example was prepared about the silicon carbide board
  • a silicon carbide single crystal substrate under the following conditions was prepared as a base substrate.
  • six 4H-type SiC single crystal substrates (three for the example and three for the comparative example) were prepared as the base substrate 1.
  • the diameter of the base substrate 1 can be in the range of 50 to 180 mm, and the thickness can be in the range of 100 to 2000 ⁇ m.
  • the thickness of the base substrate 1 is 800 ⁇ m.
  • the main surface of the base substrate 1 had an off angle of 4 ° in the ⁇ 11-20> direction with respect to the (0001) plane.
  • the surface of the base substrate 1 With respect to the surface of the base substrate 1, at least the surface on which crystals are to be grown was mirror-polished.
  • the dislocation density of the base substrate 1 micropipe density (MPD) is 10 ⁇ 100 cm -2
  • the etch pit density (EPD) was 1 ⁇ 5E4cm -2.
  • these dislocation densities were measured as follows. That is, after immersing the base substrate 1 in KOH heated to 500 ° C. for 1 to 10 minutes, the surface of the base substrate was observed with a Nomarski differential interference microscope, and the number of pits was counted. Then, the number of pits per unit area was calculated from the area of the observed area and the count number.
  • the silicon carbide ingot of the example was manufactured by forming a silicon carbide epitaxial layer on the surface of the base substrate for the example described above. Specifically, the base substrate 1 and powdered SiC as a raw material were introduced into a crucible made of graphite. The distance between the raw material and the base substrate was in the range of 10 mm to 100 mm.
  • the growth method is generally manufactured by a method called a sublimation method or a modified Rayleigh method. Specifically, the crucible was placed inside a heating furnace and heated. At the time of temperature rise, the atmospheric pressure was in the range of 50 kPa to atmospheric pressure.
  • the temperature at the time of crystal growth was in the range of 2200 ° C. or more and 2500 ° C. or less in the crucible lower temperature and 2000 ° C. or more and 2350 ° C. or less in the crucible upper portion temperature.
  • the temperature of the lower part of the heel was higher than the upper part of the heel.
  • the atmospheric pressure is controlled in the range of 0.1 to 20 kPa after the temperature is raised to the temperature at the crystal growth.
  • the atmosphere gas any one or a plurality of mixed gases of He, Ar and N 2 were used.
  • Ar + N 2 gas was used as the atmosphere gas.
  • the atmospheric pressure was first raised to the range of 50 kPa to atmospheric pressure, and then the temperature of the heating furnace was lowered.
  • the growth outermost surface of the ingot 10 grown on the surface of the base substrate 1 (the surface opposite to the side where the base substrate 1 is located in the ingot 10 of FIG.
  • the ingot 10 is grown such that the surface of the ingot 10 facing in the supply direction of the source gas to be drawn is always flat as shown in FIG.
  • the relationship is Tc.
  • the temperature gradient ((absolute value of difference between temperature Ta and temperature Tb) / (between central portion 14 and end portion 15) is satisfied for the temperature Tb and the temperature Ta.
  • Crystal growth was carried out so that the relationship (distance) would be 10 ° C./cm or less. Specifically, the diameter of the heat radiation hole of the felt located on the upper surface side of the crucible was made larger than the diameter of the ingot 10. An ingot in which silicon carbide was grown on the base substrate was taken out by this method.
  • the silicon carbide ingot of a comparative example was manufactured by forming a silicon carbide epitaxial layer on the surface of the base substrate for a comparative example.
  • the ingot of the comparative example was manufactured by the same method as the method of manufacturing the ingot of the embodiment described above, but the felt is directly disposed on the upper surface of the crucible, and the diameter of 20 mm is at the center of the felt. Heat dissipation holes were formed. By doing so, the heat radiation effect is enhanced only in the vicinity of the heat radiation holes, so the temperature gradient between the center portion 14 and the end portion 15 of the formed ingot is 10 ° C./cm or more. Thus, the ingot of the comparative example which silicon carbide grew was taken out.
  • the flatness of the surface was measured for the ingots of the examples and comparative examples described above.
  • the flatness of the ingot is the height of the ingot (from the surface of the base substrate to the surface of the ingot) in a region (at the center) excluding the range of 10% with respect to the diameter of the ingot on the outer peripheral side. Distance) was determined. Although it is preferable to take the height distribution over the entire surface of the ingot, it is sufficient to measure the height of the ingot at a pitch of 1 to 5 mm in the cross direction from the center of the ingot.
  • the flatness is measured as follows. That is, the height of the surface of the ingot 10 is measured at a plurality of positions (measurement points) arranged in a cross direction (preferably, 5 mm pitch matrix) at a pitch of 5 mm from the center of the surface of the ingot. Then, the difference in height is calculated between adjacent measurement points. Further, an angle (inclination angle) corresponding to the inclination of the surface of the ingot between adjacent measurement points is determined from the tangent (tan) which can be determined from the difference in height and the distance between the measurement points.
  • Substrate Production After measuring the surface shape as described above, the ingots of the examples and comparative examples described above were formed into a cylindrical shape. Then, a silicon carbide substrate was manufactured by slicing the ingot in the direction along the surface of the base substrate using a wire saw. The thickness of the substrate was 400 ⁇ m to 500 ⁇ m. Furthermore, after slicing, the silicon carbide substrate was subjected to double-sided mirror polishing. As a result, the thickness of the silicon carbide substrate was in the range of 350 ⁇ m to 420 ⁇ m.
  • the nitrogen concentration of the produced substrate was measured for the region located under the (0001) facet of the ingot and having a relatively high nitrogen concentration (high nitrogen concentration region) and the other regions.
  • SIMS secondary ion mass spectrometry
  • measurement thickness was 10 micrometers.
  • the light transmittance was measured for the high concentration nitrogen region and the other regions.
  • a visible light spectrometer was used to measure the transmittance of light having a wavelength of 400 nm to 500 nm.
  • the dislocation density on the surface was measured for the prepared substrate. Specifically, the following method was used. First, the silicon carbide substrate was immersed in a molten salt KOH solution heated to 500 ° C. for 1 to 10 minutes. Thereafter, the surface of the silicon carbide substrate was observed with a Nomarski differential interference microscope, and the number of pits formed was counted. It is preferable to count the total number of pits after counting the entire surface mapping photograph and to calculate the average density per unit area.
  • the number of pits per unit area is counted at a total of five points in the center of the substrate and at a distance of about 18 mm in cross direction, and the average is taken The average density of pits at five or more measurement points may be used as the density of pits.
  • the evaluated silicon carbide substrate selected the board
  • the (0001) facet is disposed on the outermost surface of the end (upstream end) in the off-angle direction of the base substrate.
  • the width of the (0001) facet in the off-angle direction in plan view is 12.5 mm for the ingot diameter 163 mm, 11 mm for the ingot diameter 115 mm, and 5.5 mm for the ingot diameter 63 mm.
  • the ingot height was also an average value when the ingot diameter was 163 mm: 13 mm, the ingot diameter 115 mm: 8 mm, and the ingot diameter 63 mm: 4 mm.
  • the inclination angle which shows the flatness of the surface of all was 10 degrees or less on average, and there was sufficient flatness.
  • the (0001) facet was generated at the center of the outermost surface of the ingot.
  • the width of the (0001) facet in the off-angle direction was in the range of 12% to 45% of the ingot diameter.
  • the inclination angle which shows the flatness of the surface exceeded 10 degrees on average.
  • the high concentration nitrogen region having a relatively high nitrogen concentration was formed in the region located under the (0001) facet (region located at the end of the substrate).
  • the arrangement of the high concentration nitrogen region almost coincided with the position of the facet.
  • the width of the high concentration nitrogen region was generally in the range of 3 to 9.5% with respect to the ingot diameter.
  • the high concentration nitrogen region was formed in the region located under the (0001) facet (the region located in the central part of the substrate).
  • the high concentration nitrogen region of the comparative example also almost coincided with the position of the facet.
  • the distribution of the size of the high concentration nitrogen region exists in the height direction of the ingot, and the width of the high concentration nitrogen region is in the range of 5 to 45% with respect to the diameter of the ingot.
  • the width (size) of the high concentration region was 10% or less with respect to the ingot diameter, but this was a region of 5 mm or less from the surface position of the base substrate. This is because, within this range, the flatness of the surface of the grown silicon carbide is relatively maintained because the total growth amount of silicon carbide is still small, and the flatness is always maintained during crystal growth. The result is different from the example.
  • the nitrogen concentration in the high concentration nitrogen region was 1.2E19 cm ⁇ 3
  • the nitrogen concentration in the other regions was 8E18 to 1E19 cm ⁇ 3
  • region was in the range of 20% with respect to the average concentration in the said 5 points
  • the nitrogen concentration in the high concentration nitrogen region was 1.2E19 cm ⁇ 3
  • the nitrogen concentration in the other region was 8E18 to 1E19 cm ⁇ 3 .
  • the transmittance of light having a wavelength of 400 to 500 nm was 10 to 20% in the high concentration nitrogen region for the substrates of Examples and Comparative Examples. Further, in the other region of the substrate, the transmittance was 25 to 35%. In addition, regarding the silicon carbide substrate cut out from the low nitrogen-doped ingot different from this experiment, the transmittance in the high concentration nitrogen region is 35 to 45%, and in the other region, the transmittance is 45 to 65%. The In addition, the refractive index of each of the silicon carbide substrates, which is obtained by calculation from the wavelength characteristic of the transmittance, was 2.5 to 2.8.
  • dislocation density The measurement was performed on a substrate obtained by slicing at a position at a distance of 20 mm from the base substrate in the ingot.
  • the dislocation density of the base substrate the micropipe density (MPD): 10 ⁇ 100cm -2
  • etch pit density (EPD) when it is 1 ⁇ 5E4cm -2
  • both MPD and EPD could be reduced to 1/2 to 1/20 of the base substrate.
  • the present invention is particularly advantageously applied to a method for manufacturing a silicon carbide ingot and a silicon carbide substrate.

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WO2024162069A1 (ja) * 2023-02-02 2024-08-08 住友電気工業株式会社 炭化珪素基板、炭化珪素エピタキシャル基板の製造方法および炭化珪素半導体装置の製造方法

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JP2015098420A (ja) * 2013-11-20 2015-05-28 住友電気工業株式会社 炭化珪素インゴットおよび炭化珪素基板の製造方法
US10711369B2 (en) 2014-12-05 2020-07-14 Showa Denko K.K. Method for producing silicon carbide single crystal and silicon carbide single crystal substrate
KR102106722B1 (ko) 2015-07-29 2020-05-04 쇼와 덴코 가부시키가이샤 에피택셜 탄화규소 단결정 웨이퍼의 제조 방법
JP6729605B2 (ja) * 2016-02-09 2020-07-22 住友電気工業株式会社 炭化珪素単結晶基板
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JP7393900B2 (ja) * 2019-09-24 2023-12-07 一般財団法人電力中央研究所 炭化珪素単結晶ウェハ及び炭化珪素単結晶インゴットの製造方法
KR102234002B1 (ko) * 2019-10-22 2021-03-29 에스케이씨 주식회사 탄화규소 잉곳, 이의 제조방법 및 탄화규소 웨이퍼의 제조방법
CN114264652B (zh) * 2021-12-09 2024-11-29 浙江大学杭州国际科创中心 碳化硅中位错产生及演变的逆向分析方法
JP2024053501A (ja) * 2022-10-03 2024-04-15 一般財団法人電力中央研究所 炭化珪素単結晶の製造方法及び炭化珪素単結晶インゴット
JP7852690B2 (ja) * 2023-12-28 2026-04-28 株式会社レゾナック ＳｉＣインゴット及びＳｉＣ基板の製造方法
JP7852691B2 (ja) * 2023-12-28 2026-04-28 株式会社レゾナック ＳｉＣインゴット、ＳｉＣ基板の製造方法およびＳｉＣインゴットの評価方法
KR20250103414A (ko) * 2023-12-28 2025-07-07 가부시끼가이샤 레조낙 SiC 잉곳 및 SiC 기판의 제조 방법

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WO2024162069A1 (ja) * 2023-02-02 2024-08-08 住友電気工業株式会社 炭化珪素基板、炭化珪素エピタキシャル基板の製造方法および炭化珪素半導体装置の製造方法

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