WO2020235225A1 - 炭化珪素基板 - Google Patents

炭化珪素基板 Download PDF

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Publication number
WO2020235225A1
WO2020235225A1 PCT/JP2020/015006 JP2020015006W WO2020235225A1 WO 2020235225 A1 WO2020235225 A1 WO 2020235225A1 JP 2020015006 W JP2020015006 W JP 2020015006W WO 2020235225 A1 WO2020235225 A1 WO 2020235225A1
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WIPO (PCT)
Prior art keywords
main surface
silicon carbide
carbide substrate
area
region
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PCT/JP2020/015006
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English (en)
French (fr)
Japanese (ja)
Inventor
恭子 沖田
翼 本家
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Priority to JP2021520639A priority Critical patent/JPWO2020235225A1/ja
Priority to US17/611,139 priority patent/US12071708B2/en
Priority to CN202080034953.3A priority patent/CN113811643B/zh
Publication of WO2020235225A1 publication Critical patent/WO2020235225A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P70/00—Cleaning of wafers, substrates or parts of devices
    • H10P70/10—Cleaning before device manufacture, i.e. Begin-Of-Line process
    • H10P70/15—Cleaning before device manufacture, i.e. Begin-Of-Line process by wet cleaning only
    • 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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D62/00—Semiconductor bodies, or regions thereof, of devices having potential barriers
    • H10D62/60—Impurity distributions or concentrations
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D62/00—Semiconductor bodies, or regions thereof, of devices having potential barriers
    • H10D62/80—Semiconductor bodies, or regions thereof, of devices having potential barriers characterised by the materials
    • H10D62/83—Semiconductor bodies, or regions thereof, of devices having potential barriers characterised by the materials being Group IV materials, e.g. B-doped Si or undoped Ge
    • H10D62/832—Semiconductor bodies, or regions thereof, of devices having potential barriers characterised by the materials being Group IV materials, e.g. B-doped Si or undoped Ge being Group IV materials comprising two or more elements, e.g. SiGe
    • H10D62/8325—Silicon carbide
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P90/00—Preparation of wafers not covered by a single main group of this subclass, e.g. wafer reinforcement
    • H10P90/12—Preparing bulk and homogeneous wafers
    • H10P90/128—Preparing bulk and homogeneous wafers by edge treatment, e.g. chamfering
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P90/00—Preparation of wafers not covered by a single main group of this subclass, e.g. wafer reinforcement
    • H10P90/12—Preparing bulk and homogeneous wafers
    • H10P90/129—Preparing bulk and homogeneous wafers by polishing
    • 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

Definitions

  • Patent Document 1 describes a method for cleaning a silicon carbide substrate.
  • the silicon carbide substrate according to the present disclosure has a main surface.
  • the maximum diameter is 150 mm or more.
  • the total area of the region where the concentrations of sodium, aluminum, potassium, calcium, titanium, iron, copper and zinc are less than 5 ⁇ 10 10 atoms / cm 2 is 95% or more of the area of the main surface. is there.
  • FIG. 1 is a schematic plan view showing the configuration of the silicon carbide substrate according to the present embodiment.
  • FIG. 2 is a schematic cross-sectional view taken along the line II-II of FIG.
  • FIG. 3 is a schematic plan view showing a measurement region of metal impurities.
  • FIG. 4 is a flowchart schematically showing a method for manufacturing a silicon carbide substrate according to the present embodiment.
  • FIG. 5 is a schematic cross-sectional view showing the first step of the method for manufacturing a silicon carbide substrate according to the present embodiment.
  • FIG. 6 is a schematic cross-sectional view showing a second step of the method for manufacturing a silicon carbide substrate according to the present embodiment.
  • An object of the present disclosure is to provide a silicon carbide substrate having high cleanliness. [Effect of this disclosure] According to the present disclosure, it is possible to provide a silicon carbide substrate having high cleanliness. [Explanation of Embodiments of the present disclosure] First, the embodiments of the present disclosure will be listed and described.
  • the silicon carbide substrate 100 includes a main surface 1.
  • the maximum diameter is 150 mm or more.
  • the total area of the region on the main surface 1 where the concentrations of sodium, aluminum, potassium, calcium, titanium, iron, copper and zinc are less than 5 ⁇ 10 10 atoms / cm 2 is 95% of the area of the main surface 1. That is all.
  • the total area may be 98% or more of the area of the main surface 1.
  • sulfur may be present on the main surface 1.
  • the region where the sulfur concentration is 5 ⁇ 10 10 atoms / cm 2 or more may be 1% or more of the area of the main surface 1.
  • the region where the sulfur concentration is 5 ⁇ 10 10 atoms / cm 2 or more may be 50% or more of the area of the main surface 1.
  • chlorine may be present on the main surface 1.
  • the region where the chlorine concentration is 5 ⁇ 10 10 atoms / cm 2 or more may be 1% or more of the area of the main surface 1.
  • the region where the chlorine concentration is 5 ⁇ 10 10 atoms / cm 2 or more may be 50% or more of the area of the main surface 1.
  • the region where the aluminum concentration is 1 ⁇ 10 12 areas / cm 2 or more is the main surface. It may be less than 1% of the area of 1.
  • the region where the potassium concentration is 1 ⁇ 10 12 areas / cm 2 or more is the main surface. It may be less than 1% of the area of 1.
  • the region where the calcium concentration is 1 ⁇ 10 12 areas / cm 2 or more is the main surface. It may be less than 1% of the area of 1.
  • FIG. 1 is a schematic plan view showing the configuration of the silicon carbide substrate 100 according to the present embodiment.
  • FIG. 2 is a schematic cross-sectional view taken along the line II-II of FIG.
  • the silicon carbide substrate 100 mainly has a first main surface 1, a second main surface 2, and a chamfered portion 6.
  • the second main surface 2 is on the opposite side of the first main surface 1.
  • the chamfered portion 6 is connected to each of the first main surface 1 and the second main surface 2.
  • Each of the first main surface 1 and the second main surface 2 is a flat surface.
  • the first main surface 1 is a surface on which an epitaxial layer (not shown) is formed.
  • the silicon carbide substrate 100 is composed of, for example, a polytype 4H hexagonal silicon carbide single crystal.
  • the silicon carbide substrate 100 contains n-type impurities such as nitrogen.
  • the first main surface 1 is, for example, a surface that is 8 ° or less off with respect to the ⁇ 0001 ⁇ surface or the ⁇ 0001 ⁇ surface. Specifically, the first main surface 1 is, for example, a surface off from the (0001) surface or the (0001) surface by 8 ° or less. The first main surface 1 may be, for example, a surface that is 8 ° or less off from the (000-1) surface or the (000-1) surface. When the first main surface 1 is the (0001) surface, the second main surface 2 is the (000-1) surface.
  • the chamfered portion 6 has a first curved region 3, an outer peripheral end portion 5, and a second curved region 4.
  • the first curved region 3 is connected to the first main surface 1.
  • the first curved region 3 is located outside the first main surface 1.
  • the second curved region 4 is connected to the second main surface 2.
  • the second curved region 4 is located outside the second main surface 2.
  • in the cross section perpendicular to the first main surface 1, each of the first curved region 3 and the second curved region 4 has an arc shape.
  • Each of the first curved region 3 and the second curved region 4 is curved so as to project outward.
  • the outer peripheral end portion 5 is a portion located on the outermost side in the radial direction parallel to the first main surface 1.
  • the outer peripheral end portion 5 is connected to each of the first curved region 3 and the second curved region 4.
  • the first curved region 3 is located between the first main surface 1 and the outer peripheral end portion 5.
  • the second curved region 4 is located between the second main surface 2 and the outer peripheral end portion 5.
  • the outer peripheral end portion 5 has an orientation flat portion 7 and an arc-shaped portion 8.
  • the arcuate portion 8 is connected to the orientation flat portion 7.
  • the orientation flat portion 7 extends along the first direction 101.
  • Each of the first direction 101 and the second direction 102 is parallel to the first main surface 1.
  • the second direction 102 is a direction perpendicular to the first direction 101.
  • the first direction 101 is, for example, the ⁇ 11-20> direction.
  • the second direction 102 is, for example, the ⁇ 1-100> direction.
  • the first direction 101 may be, for example, a direction in which the ⁇ 11-20> direction is projected onto the first main surface 1.
  • the second direction 102 may be, for example, a direction in which the ⁇ 1-100> direction is projected onto the first main surface 1.
  • the maximum diameter (first width W1) of the silicon carbide substrate 100 is 150 mm or more.
  • the maximum diameter of the silicon carbide substrate 100 when viewed in the direction perpendicular to the first main surface 1 may be calculated as the diameter of a circle including the arcuate portion 8.
  • the first width W1 may be 200 mm or more, or 250 mm or more.
  • the upper limit of the first width W1 is not particularly limited, but may be, for example, 300 mm or less.
  • the width of the chamfered portion 6 (second width W2) is, for example, 2 mm or more and 3 mm or less when viewed in the direction perpendicular to the first main surface 1.
  • the distance from the boundary between the first main surface 1 and the chamfered portion 6 to the outer peripheral end portion 5 is, for example, 2 mm or more and 3 mm or less when viewed in the direction perpendicular to the first main surface 1. ..
  • the concentration of metal impurities on the first main surface 1 will be described.
  • the total area of the region where the respective concentrations of copper (Cu) and zinc (Zn) are less than 5 ⁇ 10 10 atoms / cm 2 may be 95% or more of the area of the first main surface 1.
  • the total area of the region where each concentration of (Zn) is 5 ⁇ 10 10 atoms / cm 2 or more may be less than 5% of the area of the main surface 1. That is, the concentration of metal impurities is low in the region of 95% or more of the first main surface 1.
  • the total area of the region on the first main surface 1 where the concentrations of sodium, aluminum, potassium, calcium, titanium, iron, copper and zinc are less than 5 ⁇ 10 10 atoms / cm 2 is the main surface 1. It may be 98% or more of the area of 98.5% or more. From another point of view, on the first main surface 1, sodium (Na), aluminum (Al), potassium (K), calcium (Ca), titanium (Ti), iron (Fe), copper (Cu) and zinc.
  • the total area of the region where each concentration of (Zn) is 5 ⁇ 10 10 atoms / cm 2 or more may be less than 2% or less than 1.5% of the area of the main surface 1. Good.
  • Sulfur may be present on the first main surface 1.
  • the region where the sulfur (S) concentration is 5 ⁇ 10 10 atoms / cm 2 or more may be 1% or more of the area of the first main surface 1.
  • the region where the sulfur concentration is 5 ⁇ 10 10 atoms / cm 2 or more may be 25% or more, 50% or more, or 60% or more of the area of the first main surface 1. There may be.
  • the lower limit of the region where the sulfur concentration is 5 ⁇ 10 10 atoms / cm 2 or more is not particularly limited, but may be, for example, 75% or less of the area of the first main surface 1.
  • the region where the sulfur (S) concentration is 1 ⁇ 10 12 atoms / cm 2 or more may be 1% or more of the area of the first main surface 1.
  • the region where the sulfur concentration is 1 ⁇ 10 12 atoms / cm 2 or more may be 25% or more, 50% or more, or 60% or more of the area of the first main surface 1. There may be.
  • the lower limit of the region where the sulfur concentration is 1 ⁇ 10 12 atoms / cm 2 or more is not particularly limited, but may be, for example, 75% or less of the area of the first main surface 1.
  • Chlorine may be present on the first main surface 1.
  • the region where the chlorine (Cl) concentration is 5 ⁇ 10 10 atoms / cm 2 or more may be 1% or more of the area of the first main surface 1.
  • the region where the chlorine concentration is 5 ⁇ 10 10 atoms / cm 2 or more may be 25% or more of the area of the first main surface 1 or 50% or more of the area of the first main surface 1. It may be 60% or more of the area of the first main surface 1.
  • the lower limit of the region where the chlorine concentration is 5 ⁇ 10 10 atoms / cm 2 or more is not particularly limited, but may be, for example, 75% or less of the area of the first main surface 1.
  • the region where the chlorine (Cl) concentration is 1 ⁇ 10 12 atoms / cm 2 or more may be 1% or more of the area of the first main surface 1.
  • the region where the chlorine concentration is 1 ⁇ 10 12 atoms / cm 2 or more may be 25% or more of the area of the first main surface 1 or 50% or more of the area of the first main surface 1. It may be 60% or more of the area of the first main surface 1.
  • the lower limit of the region where the chlorine concentration is 1 ⁇ 10 12 atoms / cm 2 or more is not particularly limited, but may be, for example, 75% or less of the area of the first main surface 1.
  • the region where the aluminum concentration is 1 ⁇ 10 12 atoms / cm 2 or more may be less than 1% of the area of the first main surface 1. In the first main surface 1, there may be no region where the concentration of aluminum is 1 ⁇ 10 12 atoms / cm 2 or more.
  • the region where the potassium concentration is 1 ⁇ 10 12 atoms / cm 2 or more may be less than 1% of the area of the first main surface 1. On the first main surface 1, there may be no region where the potassium concentration is 1 ⁇ 10 12 atoms / cm 2 or more.
  • the region where the calcium concentration is 1 ⁇ 10 12 atoms / cm 2 or more may be less than 1% of the area of the first main surface 1. On the first main surface 1, there may be no region where the calcium concentration is 1 ⁇ 10 12 atoms / cm 2 or more.
  • the concentration of metal impurities can be measured by a total reflection fluorescent X-ray analyzer.
  • the analyzer for example, TXRF-3760 manufactured by Rigaku Co., Ltd. can be used.
  • the analyzer has a plurality of excitation X-ray sources, and can measure from Na as a light element to U as a heavy element by using the excitation X-rays most suitable for the measurement element.
  • W-Ma (1.78 keV) excited X-rays are used for Na, Al and Mg.
  • W-Lb (9.67 keV).
  • Excited X-ray is used.
  • the X-ray power is, for example, 35 kV-255 mA.
  • the incident direction is 39 °.
  • the incident angle of W-Ma is 0.500 °.
  • the measurement time of W-Ma is 10 seconds / point.
  • the incident angle of W-Lb is 0.100 °.
  • the measurement time of W-Lb is 10 seconds / point.
  • the analyzer has an XY drive stage and can measure the in-plane distribution of the measurement element.
  • the first main surface 1 can be divided into 101 regions with equal areas, and the concentration of the measurement element can be measured at the 101 regions.
  • the concentration of metal impurities is the number of atoms per unit area.
  • FIG. 3 is a schematic plan view showing a measurement region of metal impurities.
  • the first main surface 1 has a center 10, a first virtual circle 21, a second virtual circle 22, a third virtual circle 23, a fourth virtual circle 24, and a fifth virtual circle. It has a circle 25.
  • the distance between the first virtual circle 21 and the second virtual circle 22 is the same as the distance between the second virtual circle 22 and the third virtual circle 23.
  • the distance between the second virtual circle 22 and the third virtual circle 23 is the same as the distance between the third virtual circle 23 and the fourth virtual circle 24.
  • the distance between the third virtual circle 23 and the fourth virtual circle 24 is the same as the distance between the fourth virtual circle 24 and the fifth virtual circle 25.
  • the circles having dots represent the measurement region S of metal impurities.
  • the size of the measurement area S is 10 mm ⁇ .
  • the measurement regions S are provided at equal intervals along a straight line passing through the center 10 of the first main surface 1 and parallel to the first direction 101.
  • the measurement regions S are provided at equal intervals along a straight line passing through the center 10 of the first main surface 1 and parallel to the second direction 102.
  • One measurement area S is provided at the center 10 of the first main surface 1.
  • Eight measurement areas S are provided at equal intervals along the first virtual circle 21.
  • 16 measurement areas S are provided at equal intervals along the second virtual circle 22.
  • Twenty measurement areas S are provided at equal intervals along the third virtual circle 23.
  • Twenty-four measurement areas S are provided at equal intervals along the fourth virtual circle 24.
  • the measurement areas S are provided at 32 points at equal intervals along the fifth virtual circle 25. That is, a total of 101 measurement regions S are provided on the first main surface 1.
  • the concentrations of sodium (Na), aluminum (Al), potassium (K), calcium (Ca), titanium (Ti), iron (Fe), copper (Cu) and zinc (Zn) are measured.
  • the concentrations of sodium (Na), aluminum (Al), potassium (K), calcium (Ca), titanium (Ti), iron (Fe), copper (Cu) and zinc (Zn) are It is determined whether it is less than 5 ⁇ 10 10 atoms / cm 2 .
  • sodium (Na), aluminum (Al), potassium (K), calcium (Ca), titanium (Ti), iron (Fe), copper (Cu). ) And zinc (Zn) are measured.
  • concentrations of sodium (Na), aluminum (Al), potassium (K), calcium (Ca), titanium (Ti), iron (Fe), copper (Cu) and zinc (Zn) are It is determined whether it is less than 5 ⁇ 10 10 atoms / cm 2 .
  • sodium (Na), aluminum (Al), potassium (K), calcium (Ca), titanium (Ti), iron (Fe), and copper When the respective concentrations of Cu) and zinc (Zn) are less than 5 ⁇ 10 10 atoms / cm 2 , sodium (Na), aluminum (Al), potassium (K), calcium (Ca), titanium (Ti) ), Iron (Fe), copper (Cu) and zinc (Zn) are each less than 5 ⁇ 10 10 atoms / cm 2 , and the total area of the region is defined as the area of the first main surface 1 ⁇ N / 101. It is calculated.
  • the main surface is described as the first main surface 1, but the main surface may be the second main surface 2.
  • the concentration of metal impurities on the second main surface 2 may be the same as the concentration of metal impurities on the first main surface 1.
  • the manufacturing method of the silicon carbide substrate 100 according to the present embodiment includes a crystal preparation step (S10), a slicing step (S20), a chamfering step (S25), and a double-sided machine polishing step (S30). ), Chemical mechanical polishing step (S40), sulfuric acid overwater cleaning step (S50), ammonia overwater cleaning step (S60), hydrochloric acid overwater cleaning step (S70), and hydrofluoric acid cleaning step (S80). , The drying step (S90) is included.
  • the crystal preparation step (S10) is carried out.
  • a silicon carbide ingot is formed by a sublimation method.
  • the slicing step (S20) is carried out.
  • the silicon carbide ingot is cut out on the plurality of silicon carbide substrates 100 by the saw wire.
  • the silicon carbide substrate 100 is composed of, for example, a polytype 4H hexagonal silicon carbide single crystal. As shown in FIG. 1, the silicon carbide substrate 100 has a first main surface 1, a second main surface 2, and an outer peripheral end portion 5. At this point, the chamfered portion 6 is not formed.
  • the chamfering process (S25) is carried out.
  • a grinding device (not shown) is used.
  • a diamond grindstone is used. The vicinity of the boundary between the first main surface 1 of the silicon carbide substrate 100 and the outer peripheral end portion 5 is pressed against the rotating diamond grindstone. Similarly, the vicinity of the boundary between the first main surface 1 of the silicon carbide substrate 100 and the outer peripheral end portion 5 is pressed against the rotating diamond grindstone. As a result, the chamfered portion 6 is formed on the silicon carbide substrate 100 (see FIG. 2). In the chamfering step (S25), grinding marks may be formed on the chamfered portion 6.
  • the double-sided mechanical polishing step (S30) is carried out.
  • the silicon carbide substrate 100 is arranged so that the first main surface 1 faces the first surface plate (not shown) and the second main surface 2 corresponds to the second surface plate (not shown). It is placed between the first surface plate and the second surface plate.
  • the slurry is introduced between the first main surface 1 and the first surface plate and between the second main surface 2 and the second surface plate.
  • the slurry contains, for example, diamond abrasive grains and water.
  • the diameter of the diamond abrasive grains is, for example, 1 ⁇ m or more and 3 ⁇ m or less.
  • a load is applied to the first main surface 1 by the first surface plate, and a load is applied to the second main surface 2 by the second surface plate, so that both surfaces of the silicon carbide substrate 100 are mechanically polished.
  • the chemical mechanical polishing step (S40) is carried out. Specifically, chemical mechanical polishing is performed on the first main surface 1 of the silicon carbide substrate 100.
  • colloidal silica is used as the abrasive grains.
  • a polishing solution containing permanganate is used.
  • Abrasive cloth is attached to the surface plate.
  • the polishing cloth is, for example, a non-woven fabric.
  • the processing pressure is, for example, 300 g / cm 2 .
  • the flow rate of the polishing liquid is, for example, 50 cc / min.
  • the rotation speed of the surface plate is, for example, 40 rpm.
  • the processing time is, for example, 2 hours.
  • the sulfuric acid hydrogen peroxide cleaning step (S50) is carried out.
  • an ultrasonic cleaning device is used.
  • the ultrasonic cleaning device 20 mainly includes an ultrasonic generation source 19, a first cleaning tank 12, and a second cleaning tank 13.
  • the second cleaning tank 13 is arranged on the first cleaning tank 12.
  • the second cleaning tank 13 is hung on the opening of the first cleaning tank 12.
  • the first cleaning liquid 14 (specifically, water) is contained in the first cleaning tank 12.
  • the second cleaning liquid 15 (specifically, sulfuric acid hydrogen peroxide) is contained in the second cleaning tank 13.
  • the silicon carbide substrate 100 is immersed in sulfuric acid hydrogen peroxide.
  • the ultrasonic wave generation source 19 is arranged at the bottom of the second cleaning tank 13.
  • the second cleaning tank 13 is arranged on the ultrasonic wave generation source 19.
  • the silicon carbide substrate 100 is cleaned while the sulfuric acid hydrogen peroxide is irradiated with ultrasonic waves in order to enhance the effect of removing metal impurities.
  • the frequency of ultrasonic waves is, for example, 450 kHz or more and 2 MHz or less. Ultrasound promotes a chemical reaction. This enhances the reactivity of metal impurities with sulfuric acid hydrogen peroxide. Further, due to the cavitation effect of ultrasonic irradiation, sludge containing manganese that has entered the grinding marks of the chamfered portion 6 can be effectively removed.
  • Sulfuric acid hydrogen peroxide cleaning step (S50), mainly organic substances and metal impurities are removed.
  • Sulfuric acid superwater is a solution in which sulfuric acid, hydrogen peroxide solution, and ultrapure water are mixed.
  • sulfuric acid for example, concentrated sulfuric acid having a mass percentage concentration of 96% can be used.
  • hydrogen peroxide solution for example, a hydrogen peroxide solution having a mass percentage concentration of 30% can be used. The same applies to the hydrogen peroxide solution used in the subsequent steps.
  • the volume ratio of sulfuric acid, hydrogen peroxide solution, and ultrapure water contained in sulfuric acid superwater is, for example, 10 (sulfuric acid): 1 (hydrogen peroxide solution): 1 (ulpure water) to 10 (ulpure water) :. 3 (hydrogen peroxide solution): 1 (ultrapure water).
  • the volume of sulfuric acid is 10 times the volume of ultrapure water.
  • the volume of hydrogen peroxide solution is 1 times or more and 3 times or less the volume of ultrapure water.
  • the immersion time of the silicon carbide substrate 100 is, for example, 5 minutes or more.
  • the temperature of the sulfuric acid hydrogen peroxide is, for example, room temperature.
  • ammonia hydrogen peroxide cleaning step (S60) is carried out.
  • Ammonia superwater is a solution in which an aqueous ammonia solution, a hydrogen peroxide solution, and ultrapure water are mixed.
  • an aqueous ammonia solution for example, an aqueous ammonia solution having a mass percentage concentration of 28% can be used.
  • the silicon carbide substrate 100 may be cleaned while the ammonia hydrogen peroxide is irradiated with ultrasonic waves.
  • the volume ratio of the ammonia aqueous solution, the hydrogen peroxide solution, and the ultrapure water contained in the ammonia superwater is 1 (ammonia aqueous solution): 1 (hydrogen hydrogen solution): 5 (ultrapure water) to 1 (ammonia aqueous solution). ): 1 (hydrogenated water): 10 (ultrapure water).
  • the volume of the aqueous ammonia solution is 1/10 times or more and 1/5 times or less the volume of ultrapure water.
  • the volume of hydrogen peroxide solution is 1/10 times or more and 1/5 times or less of the volume of ultrapure water.
  • the immersion time of the silicon carbide substrate 100 is, for example, 5 minutes or more.
  • the temperature of the sulfuric acid hydrogen peroxide is, for example, room temperature.
  • the hydrochloric acid hydrogen peroxide cleaning step (S70) is carried out.
  • the hydrochloric acid overwater is a solution in which hydrochloric acid, hydrogen peroxide solution, and ultrapure water are mixed.
  • hydrochloric acid for example, concentrated hydrochloric acid having a mass percentage concentration of 98% can be used.
  • the silicon carbide substrate 100 may be cleaned while the hydrochloric acid hydrogen peroxide is irradiated with ultrasonic waves.
  • the volume ratio of hydrochloric acid, hydrogen peroxide solution, and ultrapure water contained in hydrochloric acid superwater is, for example, 1 (hydrochloric acid): 1 (hydrogen peroxide solution): 5 (ultrapure water) to 1 (hydrochloric acid) :. 1 (hydrochloric acid solution): 10 (ultrapure water).
  • the volume of hydrochloric acid is 1/10 times or more and 1/5 times or less the volume of ultrapure water.
  • the volume of hydrogen peroxide solution is 1/10 times or more and 1/5 times or less of the volume of ultrapure water.
  • the immersion time of the silicon carbide substrate 100 is, for example, 5 minutes or more.
  • the temperature of the sulfuric acid hydrogen peroxide is, for example, room temperature.
  • the hydrofluoric acid cleaning step (S80) is carried out.
  • the silicon oxide film is removed by hydrofluoric acid, and the surface is terminated with fluorine.
  • the concentration of hydrofluoric acid in the mixed solution of hydrofluoric acid and ultrapure water is, for example, 10% or more and 40% or less.
  • the immersion time of the silicon carbide substrate 100 is, for example, 5 minutes or more.
  • the temperature of the sulfuric acid hydrogen peroxide is, for example, room temperature.
  • the silicon carbide substrate 100 may be cleaned while the hydrofluoric acid is irradiated with ultrasonic waves.
  • the drying step (S90) is carried out.
  • the silicon carbide substrate 100 is dried using, for example, a spin dryer 30.
  • the spin dryer 30 includes a main body 31, a lid 32, an opening 34, and an exhaust port 33.
  • the spin dryer 30 is arranged in a clean room equivalent to class 100.
  • air is passed through the opening 34 of the spin dryer 30 toward the exhaust port 33 with the lid 32 of the spin dryer 30 open.
  • the volume of the main body 31 is, for example, 127,000 cm 3 .
  • the area of the opening 34 is, for example, 2700 cm 2 .
  • the amount of air passing is, for example, 60 m 3 .
  • the silicon carbide substrate 100 is arranged on the main body 31 of the spin dryer 30, and the lid 32 is closed.
  • the silicon carbide substrate 100 rotates around a rotation axis substantially perpendicular to the first main surface 1 in a state of being decompressed through the exhaust port 33.
  • the rotation speed of the silicon carbide substrate 100 is, for example, 800 rpm.
  • the rotation time is, for example, 300 seconds.
  • the cleaning liquid adhering to the silicon carbide substrate 100 is removed by centrifugal force.
  • the cleanliness of the main surface 1 of the silicon carbide substrate 100 is often discussed by the average value of the impurity concentrations measured at a plurality of points in the main surface 1.
  • the average value will be small when discussed, and it may be judged as a non-defective product.
  • a leakage current may be generated through the impurities.
  • the silicon carbide substrate 100 is cleaned while the sulfuric acid hydrogen peroxide is irradiated with ultrasonic waves.
  • Ultrasound promotes a chemical reaction. This enhances the reactivity of metal impurities with sulfuric acid hydrogen peroxide.
  • the cavitation effect of ultrasonic irradiation can effectively remove metal impurities concentrated and adhering to a specific place. Therefore, the concentration of metal impurities can be reduced in most of the region of the main surface 1.
  • the total area of the region on the main surface 1 where the concentrations of sodium, aluminum, potassium, calcium, titanium, iron, copper and zinc are less than 5 ⁇ 10 10 atoms / cm 2 is the main surface 1. It can be 95% or more of the area of.
  • the silicon carbide substrate 100 having high cleanliness can be obtained.
  • a spin dryer may be used.
  • the dust adhering to the inside of the spin dryer, the dust generated when the spin dryer operates, or the atmosphere around the spin dryer floats.
  • the dust and the like may adhere firmly to the silicon carbide substrate 100 that is wet with the cleaning liquid used in the cleaning step.
  • the dust contains metal impurities and causes contamination of the silicon carbide substrate 100.
  • the spin dryer 30 is in a state where the lid 32 of the spin dryer 30 is opened before the silicon carbide substrate 100 is put into the spin dryer 30. A certain amount or more of air is passed from the opening 34 toward the exhaust port 33. After that, the silicon carbide substrate 100 is arranged in the spin dryer 30, and the silicon carbide substrate 100 is dried. As a result, it is possible to prevent dust containing metal impurities from adhering to the main surface 1 of the silicon carbide substrate 100. Therefore, the concentration of metal impurities can be reduced in most of the region of the main surface 1.
  • the total area of the region on the main surface 1 where the concentrations of sodium, aluminum, potassium, calcium, titanium, iron, copper and zinc are less than 5 ⁇ 10 10 atoms / cm 2 is the main surface 1. It can be 95% or more of the area of.
  • the silicon carbide substrate 100 having high cleanliness can be obtained.
  • sample preparation First, the silicon carbide substrate 100 according to sample 1 and the silicon carbide substrate 100 according to sample 2 were prepared.
  • the silicon carbide substrate 100 according to sample 1 is a comparative example.
  • the silicon carbide substrate 100 according to sample 2 is an example.
  • the maximum diameter (diameter) of the silicon carbide substrate 100 was set to 150 mm.
  • the silicon carbide substrate 100 according to Sample 2 was manufactured by the manufacturing method according to the present embodiment. Specifically, in the sulfuric acid hydrogen peroxide cleaning step (S50), ultrasonic waves were applied to the sulfuric acid hydrogen peroxide. The frequency of the ultrasonic wave was 950 kHz. The volume ratio of sulfuric acid, hydrogen peroxide solution, and ultrapure water contained in sulfuric acid superwater was 10 (sulfuric acid): 1 (hydrogen peroxide solution): 1 (ultrapure water). The immersion time of the silicon carbide substrate 100 was 30 minutes. The temperature of the sulfuric acid hydrogen peroxide was room temperature.
  • the opening 34 of the spin dryer 30 is opened with the lid 32 of the spin dryer 30 opened before the silicon carbide substrate 100 is put into the spin dryer 30. Air was passed toward the exhaust port 33. The amount of air passing through was 60 m 3 .
  • the concentration of metal impurities was measured using TXRF-3760 manufactured by Rigaku Co., Ltd.
  • the X-ray power was 35 kV-255 mA.
  • the incident direction was 39 °.
  • the incident angle of W-Ma was 0.500 °.
  • the measurement time of W-Ma was 10 seconds / point.
  • the incident angle of W-Lb was 0.100 °.
  • the measurement time of W-Lb was 10 seconds / point.
  • Table 1 shows sodium (Na), aluminum (Al), potassium (K), calcium (Ca), titanium (Ti), iron (Fe), copper (Cu), zinc (Zn), sulfur (S) and chlorine.
  • the area ratio of the measurement region S in which each concentration of (Cl) is equal to or higher than the reference value is shown.
  • the reference values were 1 ⁇ 10 12 atoms / cm 2 and 5 ⁇ 10 10 atoms / cm 2 .
  • the area ratios of the measurement area S in which the concentrations of Zn), sulfur (S) and chlorine (Cl) are 5 ⁇ 10 10 atoms / cm 2 or more are 0%, 0%, 1%, 0% and 0, respectively. %, 0%, 0%, 0%, 68% and 62%.
  • the area ratios of the measurement area S in which the concentrations of (Cu), zinc (Zn), sulfur (S) and chlorine (Cl) are 1 ⁇ 10 12 titanium / cm 2 or more are 0%, 1% and 1 respectively. %, 1%, 0%, 0%, 0%, 0%, 88% and 78%.
  • the area ratios of the measurement region S in which the concentrations of Zn), sulfur (S) and chlorine (Cl) are 1 ⁇ 10 12 titanium / cm 2 or more are 0%, 0%, 0%, 0% and 0, respectively. %, 0%, 0%, 0%, 68% and 62%.
  • the area ratio of the region where the metal impurities to be measured are equal to or more than the reference value can be reduced as compared with the silicon carbide substrate 100 according to the sample 1.

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  • Inorganic Chemistry (AREA)
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  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
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