WO2023074219A1 - 多結晶SiC成形体及びその製造方法 - Google Patents
多結晶SiC成形体及びその製造方法 Download PDFInfo
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- polycrystalline sic
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000001020 plasma etching Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims description 36
- 239000000758 substrate Substances 0.000 claims description 33
- 238000000227 grinding Methods 0.000 claims description 27
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 85
- 229910010271 silicon carbide Inorganic materials 0.000 description 84
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 25
- 239000007789 gas Substances 0.000 description 21
- 230000015572 biosynthetic process Effects 0.000 description 16
- 238000005530 etching Methods 0.000 description 15
- 229910052757 nitrogen Inorganic materials 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 9
- 229920005992 thermoplastic resin Polymers 0.000 description 7
- 235000012431 wafers Nutrition 0.000 description 7
- 235000013339 cereals Nutrition 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 241001441571 Hiodontidae Species 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
- B24B7/20—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
- B24B7/22—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
- B24B7/228—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain for grinding thin, brittle parts, e.g. semiconductors, wafers
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32532—Electrodes
- H01J37/3255—Material
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
- C04B2235/722—Nitrogen content
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/963—Surface properties, e.g. surface roughness
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/9638—Tolerance; Dimensional accuracy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/32—Processing objects by plasma generation
- H01J2237/33—Processing objects by plasma generation characterised by the type of processing
- H01J2237/334—Etching
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
Definitions
- the present invention relates to a polycrystalline SiC compact and a method for producing the same.
- Patent Document 1 Japanese Unexamined Patent Application Publication No. 2001-220237 describes that silicon carbide (SiC) is used as an electrode or the like of a plasma etching apparatus used in the manufacture of semiconductor devices.
- the area of the wafers is increasing and the density of the circuits formed is increasing. Therefore, there is a demand for a technology capable of etching semiconductor wafers in a more uniform manner, even for plasma etching performed during the manufacture of semiconductor devices.
- Patent Document 1 the uniformity of the electrical resistivity (Patent Document 1), the uniformity of the thermal conductivity, and the smoothness of the surface of the electrode are thought to affect the uniformity of the plasma etching. be done.
- Patent Document 1 the uniformity of the electrical resistivity
- the uniformity of the thermal conductivity the uniformity of the thermal conductivity
- the smoothness of the surface of the electrode are thought to affect the uniformity of the plasma etching. be done.
- SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a polycrystalline SiC compact and a method for producing the same that can achieve uniform plasma etching when used as an electrode.
- the present inventors found that the above problem can be solved by setting the arithmetic mean waviness obtained from the specific wavelength component in the waviness curve extracted from the cross-sectional curve of the main surface of the polycrystalline SiC molded body to within a specific range. rice field. That is, the present invention provides the following.
- One embodiment of the present invention is a polycrystalline SiC molded body having two opposing main surfaces, wherein the arithmetic mean waviness Wa corresponding to a predetermined wavelength range extracted from the cross-sectional curves of the main surfaces is the wavelength When the range is 0 to 10 mm, the Wa is 0.05 ⁇ m or less, and when the wavelength range is 10 to 20 mm, the Wa is 0.13 ⁇ m or less, and the wavelength range is 20 to 30 mm. It is a polycrystalline SiC compact in which the Wa is 0.20 ⁇ m or less.
- one embodiment of the present invention is the above-described method for manufacturing a polycrystalline SiC compact, comprising: forming a polycrystalline SiC film having a main surface; and grinding the main surface of the polycrystalline SiC film. and the step of grinding comprises: grinding the main surface with a first abrasive; and grinding the main surface with a second abrasive after the step of grinding with the first abrasive.
- the grain size of the first abrasive is the second
- the grain size of the second abrasive is coarser than that of the abrasive
- the grain size of the second abrasive is coarser than that of the third abrasive.
- a polycrystalline SiC compact that can achieve uniform plasma etching when used as an electrode, and a method for producing the same.
- the polycrystalline SiC compact according to this embodiment has two main surfaces facing each other.
- the two major surfaces include a first major surface and a second major surface.
- the main surface refers to a substantially flat surface.
- the arithmetic mean waviness Wa corresponding to the predetermined wavelength range extracted from the cross-sectional curve of the main surface is 0.05 ⁇ m or less when the wavelength range is 0 to 10 mm, and 0.13 ⁇ m or less when the wavelength range is 10 to 20 mm. and is 0.20 ⁇ m or less when the wavelength range is 20 to 30 mm.
- the definitions of "section curve” and "arithmetic mean waviness" conform to JIS B 0601.
- the cross-sectional curve is expanded into frequencies, and the frequency at which the amplitude transmissibility of frequency components of 1 ⁇ 10 3 /m or higher is 50% is set as the cutoff value. to derive the arithmetic mean waviness.
- the frequency expansion is preferably expansion by Fourier transform.
- the arithmetic mean waviness Wa when the wavelength range is 0 to 10 mm (hereinafter referred to as “Wa (0 to 10 mm)”) is an arithmetic Average swell.
- the arithmetic mean waviness Wa when the wavelength range is 10 to 20 mm (hereinafter referred to as "Wa (10 to 20 mm)") is obtained from the component with a spatial frequency of 1/2 to 1 ( ⁇ 10 3 /m) in the profile curve. is the calculated arithmetic mean swell.
- the arithmetic mean waviness Wa when the wavelength range is 20 to 30 mm (hereinafter referred to as "Wa (20 to 30 mm)") is a component with a spatial frequency of 1/3 to 1/2 ( ⁇ 10 3 /m) in the profile curve is the arithmetic mean swell obtained from
- a polycrystalline SiC molded body having a specific Wa (0 to 10 mm), a specific Wa (10 to 20 mm), and a specific Wa (20 to 30 mm) is used as an electrode.
- a specific Wa (0 to 10 mm)
- a specific Wa (20 to 30 mm) is used as an electrode.
- the polycrystalline SiC compact according to this embodiment has a highly flat main surface. Therefore, the polycrystalline SiC compact according to the present embodiment can be suitably used not only as an electrode for a plasma etching apparatus, but also for other applications requiring flatness.
- the polycrystalline SiC compact according to the present embodiment may be bonded to a single crystal SiC substrate and used as a supporting base material for the single crystal SiC substrate. In such applications, the polycrystalline SiC compact is required to have a flat surface.
- the polycrystalline SiC compact according to this embodiment has a flat main surface. Therefore, it can be suitably used for applications in which it is used in combination with a single crystal SiC substrate.
- the polycrystalline SiC compact is disk-shaped. That is, the main surface of the polycrystalline SiC compact is circular. More preferably, the polycrystalline SiC compact is a disk-shaped polycrystalline SiC compact, and the diameter of the main surface of the polycrystalline SiC compact is 1.5 to 20 inches, more preferably 6 to 18 inches. is.
- the thickness of the polycrystalline SiC compact is 0.1-4.0 mm.
- the manufacturing method according to the present embodiment includes a step of forming a polycrystalline SiC film having a main surface (step S1) and a step of grinding the main surface of the polycrystalline SiC film (step S2). Each step will be described in detail below.
- Step S1 Formation of Polycrystalline SiC Film
- a polycrystalline SiC film can be formed using, for example, the CVD method.
- the film formation conditions are not particularly limited, and known conditions (for example, Japanese Unexamined Patent Application Publication No. 2021-54666) can be employed.
- a graphite substrate or the like is placed as a base material in a CVD furnace.
- a carrier gas, a raw material gas serving as a supply source of SiC, and a nitrogen-containing gas are mixed as necessary, and the mixed gas is supplied to the CVD furnace.
- the surface temperature of the substrate is set so that polycrystalline SiC is produced from the raw material gas. Thereby, a polycrystalline SiC layer is formed on the substrate.
- the polycrystalline SiC layer can be doped with nitrogen. After deposition of the polycrystalline SiC layer, the resulting polycrystalline SiC layer is separated from the substrate. Thereby, a polycrystalline SiC film having two main surfaces (that is, a first main surface and a second main surface) is obtained.
- the polycrystalline SiC film obtained above preferably has a volume resistivity of 0.050 ⁇ cm or less.
- the volume resistivity of the polycrystalline SiC film is such that when it is used as an electrode for plasma etching, it is possible to effectively release static electricity and generate plasma gas uniformly. can.
- the volume resistivity of the polycrystalline SiC film is preferably 0.030 ⁇ cm or less, more preferably 0.020 ⁇ cm or less, from the viewpoint of ensuring a high etching rate when used as a plasma etching electrode.
- the volume resistivity can be adjusted, for example, by adding a predetermined amount of nitrogen to the polycrystalline SiC film. Volume resistivity can be lowered by increasing the nitrogen content.
- the nitrogen content of the polycrystalline SiC film is, for example, 200 ppm (parts per million mass) or more, preferably 200 to 1000 ppm (parts per million mass).
- the nitrogen content is in this range, the degree of change in resistivity with respect to the change in nitrogen content is small. Therefore, controlling the nitrogen content of the polycrystalline SiC film facilitates obtaining a desired volume resistivity.
- the nitrogen content is 1000 ppm (parts per million by mass) or less, the crystal defects caused by the introduction of nitrogen hardly affect the flatness of the polycrystalline SiC film.
- the method of introducing nitrogen is not particularly limited. For example, as described above, nitrogen can be introduced into the formed polycrystalline SiC film by using a nitrogen-containing gas when forming the polycrystalline SiC film by the CVD method.
- Step S2 Grinding Subsequently, the two main surfaces of the obtained polycrystalline SiC film are ground.
- the main surface is ground in three steps (steps S2-1 to S2-3) described below.
- Step S2-1 the main surface of the polycrystalline SiC film is ground with a first abrasive.
- the polycrystalline SiC film is placed on a support substrate (for example, a flat metal plate) and fixed to the support substrate with a first fixing material.
- the polycrystalline SiC film is fixed to the support substrate so that one main surface side is released.
- the main surface of the released polycrystalline SiC film is ground with a first abrasive.
- the polycrystalline SiC substrate is removed from the support substrate.
- the other main surface is similarly ground.
- the second main surface may be ground.
- the first main surface may be ground.
- the polycrystalline SiC film is fixed on the support substrate, for example, by the following procedure.
- a fixing material for example, thermoplastic resin
- the fixing material is softened by heat conducted from the hot plate, and the polycrystalline SiC film is adhered to the supporting substrate.
- the heating of the hot plate is stopped, the supporting substrate and the polycrystalline SiC film fixed thereon are cooled, the fixing material is cured, and the polycrystalline SiC film is fixed on the supporting substrate.
- the first abrasive for example, a cup grindstone or abrasive fine powder can be used.
- abrasive fine powder an abrasive having a relatively coarse particle size (for example, #50 to #500) is used.
- the definition of "granularity" conforms to JIS R 6001-1 and JIS R 6001-2.
- a thermoplastic resin is used as the first fixing material.
- the first fixing material it is preferable to use one having a Mooney viscosity of 30 to 60M.
- Mooney viscosity is expressed in Mooney units (M).
- Mooney unit is a unit indicated or recorded by a torque indicating device used in a viscosity test and a Mooney scorch test in accordance with JIS K 6300-1. Specifically, when the torque acting on the shaft of the rotor is 8.30 N ⁇ m, it is called 100 Mooney units (100M).
- Step S2-2 Subsequently, the polycrystalline SiC film is removed from the support substrate, and the first fixing material on the support substrate is removed. After that, the polycrystalline SiC film is fixed on the supporting substrate by the second fixing material in the same manner as in step S2-1. Next, the main surface of the polycrystalline SiC film is ground with a second abrasive.
- the second abrasive a cup whetstone or polishing fine powder can be used as in the case of the first abrasive.
- the grain size of the second abrasive is finer than the grain size of the first abrasive.
- the particle size of the second abrasive is, for example, greater than #500 and equal to or less than #5000 in the case of fine abrasive powder.
- thermoplastic resin or the like can be used as the second fixing member, like the first fixing member.
- the second fixing material one having a Mooney viscosity higher than that of the first fixing material is preferably used.
- the Mooney viscosity of the second fixing material is, for example, 60-80M.
- step S2-2 the polycrystalline SiC film is removed from the support substrate, and the second fixing material on the support substrate is removed. After that, the polycrystalline SiC film is fixed on the supporting substrate by the third fixing material in the same manner as in step S2-1. Next, the main surface of the polycrystalline SiC film is ground with a third abrasive.
- the third abrasive like the first and second abrasives, a cup whetstone or polishing fine powder can be used.
- the particle size of the third abrasive is finer than that of the second abrasive.
- the particle size of the third abrasive is, for example, greater than #5000 and equal to or less than #50000 in the case of fine abrasive powder.
- the third fixing member a thermoplastic resin or the like can be used as in the case of the first and second fixing members.
- the Mooney viscosity of the third fixing material is preferably higher than that of the second fixing material.
- the Mooney viscosity of the third fixing material is, for example, 80-120M.
- the grinding process of steps S2-1 to 2-3 is performed by changing the abrasive material and the fixing material.
- both the unevenness (spatial frequency: low) between positions separated by a certain distance on the main surface of the polycrystalline SiC film and the unevenness of the morphology between adjacent precipitated grains (spatial frequency: high) are flattened.
- a polycrystalline SiC compact having a specific Wa (0 to 10 mm), a specific Wa (10 to 20 mm) and a specific Wa (20 to 30 mm) can be obtained.
- a disc-shaped graphite substrate having a diameter of 220 mm and a thickness of 5 mm was placed in a CVD furnace.
- Trimethylchlorosilane as a raw material gas, hydrogen as a carrier gas, and nitrogen gas were introduced into a CVD furnace, and the substrate temperature was set to 1500° C. for 10 hours of reaction to form a polycrystalline SiC film on the graphite substrate.
- the initial stage of film formation from the start of film formation to 2.5 hours
- the middle period of film formation from 2.5 hours to 5 hours after the start of film formation
- the latter period of film formation from 5 hours to 10 hours after the start of film formation up to
- the concentration of the raw material gas was changed.
- the source gas concentration (first concentration) in the early stage of film formation was set to 9.0 vol%
- the source gas concentration (second concentration) in the latter stage of film formation was set to 7.5 vol%. That is, the ratio of the raw material gas concentration in the early stage of film formation to the raw material gas concentration in the latter stage of film formation (referred to as the raw material gas concentration ratio) was set to 1.2 times.
- the raw material gas concentration was decreased at a constant rate from the concentration at the beginning of film formation to the concentration at the latter stage of film formation.
- the raw material gas flow rate and the carrier gas flow rate were controlled so that the total value of the raw material gas flow rate and the carrier gas flow rate was constant (140 L/min.).
- the nitrogen gas flow rate was kept constant throughout the film formation period. Specifically, the nitrogen gas flow rate was set to 17.5 (L/min.).
- the graphite substrate was taken out of the CVD furnace and subjected to peripheral processing and division processing. Further, the graphite substrate was removed to obtain a disk-shaped polycrystalline SiC film with a diameter of 205 mm and a thickness of 0.6 mm.
- thermoplastic resin with a Mooney viscosity of 45M was used as the first fixing material, and polishing fine powder with an average particle size of #200 was used as the first abrasive.
- a thermoplastic resin with a Mooney viscosity of 70M was used as the second fixing material, and polishing fine powder with an average particle size of #3000 was used as the second abrasive.
- a thermoplastic resin with a Mooney viscosity of 100M was used as the third fixing material, and polishing fine powder with an average particle size of #40000 was used as the third abrasive.
- An iron-based metal flat plate with high thermal conductivity was used as a support substrate for fixing the polycrystalline SiC film during grinding.
- a polycrystalline SiC film processed for a plasma etching electrode was placed in an etching apparatus as an electrode, and a voltage was applied to generate CF 4 plasma.
- a silicon wafer having a diameter of 8 inches and a thickness of 0.5 mm was placed on a sample stage as a material to be etched, and after etching with the aforementioned CF 4 plasma for 1 hour, the thickness distribution of the silicon wafer was measured to evaluate etching unevenness.
- the evaluation index was the value of "minimum value of etching amount/maximum value of etching amount”. If this value is 0.98 or more, it is judged to be better than the prior art (A), and if it is 0.95 or more and less than 0.98, it is judged to be equivalent to the prior art (B). It was judged to be (C) inferior to the prior art in some cases.
- the volume resistivity of the polycrystalline SiC film was measured by the four-probe method. The measurement points were the center point and other arbitrary nine points on one main surface of the polycrystalline SiC film.
- the volume resistivity of the polycrystalline SiC film was taken as the arithmetic mean value of the above ten measurement values, and the degree of variation in the volume resistivity was evaluated by standard deviation.
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Abstract
Description
また、本発明の一実施形態は、上記の多結晶SiC成形体の製造方法であって、主面を有する多結晶SiC膜を成膜する工程と、前記多結晶SiC膜の主面を研削する工程と、を備え、前記研削する工程は、前記主面を、第1の研削材により研削する工程と、前記第1の研削材により研削する工程の後に、前記主面を第2の研削材により研削する工程と、前記第2の研削材により研削する工程の後に、前記主面を第3の研削材により研削する工程とを備え、前記第1の研削材の粒度は、前記第2の研削材よりも粗く、前記第2の研削材の粒度は、前記第3の研削材よりも粗い、多結晶SiC成形体の製造方法である。
本実施形態に係る多結晶SiC成形体は、対向する2つの主面を有している。2つの主面は、第1主面及び第2主面を含む。本願明細書において、主面とは略平面を指す。この主面の断面曲線から抽出した所定の波長範囲に対応する算術平均うねりWaは、波長範囲が0~10mmのとき0.05μm以下であり、波長範囲が10~20mmのとき0.13μm以下であり、かつ、波長範囲が20~30mmのとき0.20μm以下である。
ここで、「断面曲線」及び「算術平均うねり」の定義は、JIS B 0601に準拠するものである。例えば、断面曲線から波長範囲0~10mmを抽出するときは、断面曲線を周波数展開し、1×103/m以上の周波数成分の振幅伝達率が50%となる周波数をカットオフ値に設定して、算術平均うねりを導出する。このとき、周波数展開は、フーリエ変換による展開であることが好ましい。
続いて、本実施形態に係る多結晶SiC成形体の製造方法について説明する。
本実施形態に係る製造方法は、主面を有する多結晶SiC膜を成膜する工程(ステップS1)と、前記多結晶SiC膜の主面を研削する工程(ステップS2)とを備える。以下に、各工程について詳述する。
多結晶SiC膜は、例えば、CVD法を用いて成膜することができる。成膜条件は、特に限定されるものではなく、公知の条件(例えば、特開2021-54666号公報)を採用することができる。
例えば、まず、CVD炉内に、基材として黒鉛基板等を配置する。
そして、キャリアガス、SiCの供給源となる原料ガス、及び必要に応じて窒素含有ガスを混合し、その混合ガスをCVD炉に供給する。基材の表面の温度を原料ガスから多結晶SiCが生成するように設定する。これにより、基材上に多結晶SiC層が成膜される。また、窒素含有ガスを用いた場合には、多結晶SiC層に窒素をドープすることができる。
多結晶SiC層の成膜後、得られた多結晶SiC層を基材から分離する。これにより、2つの主面(すなわち、第1主面及び第2主面)を有する多結晶SiC膜が得られる。
体積抵抗率は、例えば、多結晶SiC膜中に所定の量で窒素を含有させることにより、調整することができる。窒素含有量を増やすことにより、体積抵抗率を下げることができる。
多結晶SiC膜の窒素含有量は、例えば200ppm(質量百万分率)以上であり、好ましくは200~1000ppm(質量百万分率)である。窒素含有量がこのような範囲にある場合、窒素含有量の変化に対する抵抗率の変化の度合いが小さくなる。従って、多結晶SiC膜の窒素含有量を制御することによって、所望する体積抵抗率を得やすくなる。また、窒素含有量が1000ppm(質量百万分率)以下であれば、窒素の導入により生じる結晶欠陥が多結晶SiC膜の平坦性に影響を及ぼすこともほとんどない。
尚、窒素の導入方法は特に限定されるものでは無い。例えば、上記のように、CVD法によって多結晶SiC膜を成膜する際に、窒素含有ガスを用いることにより、成膜される多結晶SiC膜に窒素を導入することができる。
続いて、得られた多結晶SiC膜の2つの主面を研削する。ここで、主面は、以下に説明する3段階(ステップS2-1~S2-3)によって研削される。
まず、多結晶SiC膜の主面を、第1の研削材により研削する。具体的には、多結晶SiC膜を支持基板(例えば、金属平板)の上に載置し、第1の固定材で支持基板に固定する。この際、多結晶SiC膜は、一方の主面側が解放されるように支持基板に固定される。そして、解放されている多結晶SiC膜の主面を、第1の研削材により研削する。一方の主面の研削後、多結晶SiC基板を支持基板から取り外す。そして、他方の主面についても同様に研削する。第1主面の研削後に、第2主面が研削されてもよい。第2主面の研削後に、第1主面が研削されてもよい。
また、第1の研削材としては、例えば、研磨微粉の場合、比較的粗い粒度(例えば、♯50~♯500)を有する研削材が用いられる。ここで、「粒度」の定義は、JIS R 6001-1及びJIS R 6001-2に準拠するものである。
また、第1の固定材としては、ムーニー粘度が30~60Mであるものを用いることが好ましい。
ここで、ムーニー粘度は、ムーニー単位(M)で表す。ムーニー単位は、JIS K 6300-1に準拠して、粘度試験及びムーニースコーチ試験で用いるトルク指示装置によって指示又は記録する単位のことを指す。具体的には、ロータのシャフトに作用するトルクが8.30N・mのときを100ムーニー単位(100M)という。
続いて、支持基板から多結晶SiC膜を取り外し、支持基板上の第1の固定材を除去する。その後、ステップS2-1と同様の方法で、第2の固定材により多結晶SiC膜を支持基板上に固定する。次いで、第2の研削材により多結晶SiC膜の主面を研削する。
ここで、第2の研削材の粒度は、第1の研削材の粒度よりも細かい。第2の研削材の粒度は、例えば、研磨微粉の場合、♯500超、♯5000以下である。
ここで、第2の固定材としては、第1の固定材よりもムーニー粘度が大きいものが好ましく用いられる。第2の固定材のムーニー粘度は、例えば、60~80Mである。
最後に、ステップS2-2と同様に、支持基板から多結晶SiC膜を取り外し、支持基板上の第2の固定材を除去する。その後、ステップS2-1と同様の方法で、第3の固定材により多結晶SiC膜を支持基板上に固定する。次いで、第3の研削材により多結晶SiC膜の主面を研削する。
ここで、第3の研削材の粒度は、第2の研削材より細かい。第3の研削材の粒度は、例えば、研磨微粉の場合、♯5000超、♯50000以下である。
ここで、第3の固定材のムーニー粘度は、第2の固定材のそれよりも大きいことが好ましい。第3の固定材のムーニー粘度は、例えば、80~120Mである。
CVD炉内に、直径220mm、厚さ5mmの円盤状の黒鉛基板を設置した。CVD炉に、原料ガスであるトリメチルクロロシラン、キャリアガスである水素、及び窒素ガスを導入し、基板温度を1500℃に設定して10時間反応させ、黒鉛基板上に多結晶SiC膜を成膜した。
尚、成膜初期(成膜開始から2.5時間まで)と、成膜中期(成膜開始後2.5時間から5時間まで)と、成膜後期(成膜開始後5時間から10時間まで)との間において、原料ガスの濃度を変化させた。具体的には、成膜初期の原料ガス濃度(第1濃度)を9.0vol%とし、成膜後期の原料ガス濃度(第2濃度)を7.5vol%とした。
すなわち、成膜後期の原料ガス濃度に対する成膜初期の原料ガス濃度の比(原料ガス濃度比という)を、1.2倍とした。また、成膜中期においては、成膜初期の濃度から成膜後期の濃度まで、原料ガス濃度を一定の速度で低下させた。尚、原料ガス流量とキャリアガス流量との合計値が一定(140L/min.)になるように、原料ガス流量及びキャリアガス流量を制御した。
また、窒素ガス流量は、成膜期間全体を通じて、一定とした。具体的には、窒素ガス流量については、17.5(L/min.)とした。
(式1):ガス滞留時間(秒)=(炉内容積/ガス流量)×((20+273)/(反応温度+273))×60
多結晶SiC膜の主面の断面曲線、その断面曲線から3つの波長範囲(0~10mm、10~20mm、20~30mm)の抽出、及び抽出された各波長に対応する算術平均うねり(Wa(0~10mm)、Wa(10~20mm)、Wa(20~30mm))は、コーニングトロペル社製FlatMasterを用いて測定し算出した。
プラズマエッチング電極用に加工した多結晶SiC膜を電極としてエッチング装置に設置し、電圧を印加し、CF4プラズマを発生させた。φ8インチ、0.5mm厚のシリコンウエーハを被エッチング材料として試料ステージに配置し、先述のCF4プラズマで1時間エッチングした後に、シリコンウエーハの厚み分布を測定しエッチングむらを評価した。
平面度が乏しい(すなわち、算術平均うねりが大きい場合)プラズマエッチング電極の場合、均一な強度のプラズマが発生しないため、同じ時間エッチングした場合にも被エッチング材料のエッチングレートに差が生じる。従って、シリコンウエーハの厚み差が小さいほど均一な強度のプラズマが発生していることを示している。
表2は、各例についての算術平均うねりWa(0~10mm)、Wa(10~20mm)、Wa(20~30mm)及びエッチングむらの評価結果として記載した。
プラズマエッチングの前後で、被エッチング面内の任意17箇所のシリコンウエーハの厚みを測定し、被エッチング面内のエッチング量の差を評価した。ここで、評価指標は、「エッチング量の最小値/エッチング量の最大値」の値とした。この値が、0.98以上の場合に従来技術より良(A)と判断し、0.95以上0.98未満の場合に従来技術と同等と判断し(B)、また0.95未満の場合に従来技術より劣る(C)と判断した。
多結晶SiC膜の体積抵抗率は、四探針法により測定された。測定箇所は、多結晶SiC膜の一方の主面の、中心点及びその他任意の9点とした。ここで、多結晶SiC膜の体積抵抗率は、上記10点の測定値の算術平均値とし、体積抵抗率のばらつきの程度は、標準偏差で評価した。
比較例1では、ポーラスチャックのみを用いて多結晶SiC膜を固定し研削を行っている。このとき、3つの波長範囲全ての算術平均うねりの値が、実施例1~3と比べて大な値であった。ポーラスチャックのみにより固定した研削方法では、主面表面のうねりは除去できないことが分かる。さらに、比較例1の多結晶SiC膜によるプラズマエッチング電極を用いてエッチングを行ったとき、実施例1~3よりも大きなエッチングむらが生じた。
実施例1~3では、3つの波長範囲全ての算術平均うねりの値が、比較例1~5に比べて小さく、エッチングむらが小さく良好であった。実施例1~3と比較例5とを比較した場合、工程の進行に従ってムーニー粘度を大きくすることにより、高周波数のうねりの除去効果が高いことが分かった。ムーニー粘度の異なる固定材が、研削加工時に発生する研削装置の振動や装置アライメントの微小なずれに追従して、弾性変形しながら多結晶SiC膜を固定することにより、従来よりも高度にうねりを除去する効果を奏すると考えられる。
ここで、実施例1~3及び比較例1~5において、それらの体積抵抗率は、いずれも0.010Ωcm未満であった。また、それらの標準偏差は0.010未満であった。
Claims (6)
- 対向する2つの主面を有する多結晶SiC成形体であって、
前記主面の断面曲線から抽出した、所定の波長範囲に対応する算術平均うねりWaは、
前記波長範囲が、0~10mmのとき、前記Waが0.05μm以下であり、
前記波長範囲が、10~20mmのとき、前記Waが0.13μm以下であり、かつ
前記波長範囲が、20~30mmのとき、前記Waが0.20μm以下である、
多結晶SiC成形体。 - 体積抵抗率が0.050Ωcm以下である、請求項1に記載の多結晶SiC成形体。
- プラズマエッチング装置における電極として使用される、請求項1に記載の多結晶SiC成形体。
- 請求項1~3のいずれか1項に記載の多結晶SiC成形体の製造方法であって、
主面を有する多結晶SiC膜を成膜する工程と、
前記多結晶SiC膜の主面を研削する工程と、
を備え、
前記研削する工程は、
前記主面を、第1の研削材により研削する工程と、
前記第1の研削材により研削する工程の後に、前記主面を第2の研削材により研削する工程と、
前記第2の研削材により研削する工程の後に、前記主面を第3の研削材により研削する工程とを備え、
前記第1の研削材の粒度は、前記第2の研削材よりも粗く、
前記第2の研削材の粒度は、前記第3の研削材よりも粗い、
多結晶SiC成形体の製造方法。 - 前記第1の研削材により研削する工程は、第1の固定材を用いて前記多結晶SiC膜を支持基板上に固定する工程を有し、
前記第2の研削材により研削する工程は、第2の固定材を用いて前記多結晶SiC膜を前記支持基板上に固定する工程を有し、
前記第3の研削材により研削する工程は、第3の固定材を用いて前記多結晶SiC膜を前記支持基板上に固定する工程を有し、
前記第1の固定材のムーニー粘度は、前記第2の固定材のムーニー粘度より小さく、
前記第2の固定材のムーニー粘度は、前記第3の固定材のムーニー粘度より小さい、
請求項4に記載の多結晶SiC成形体の製造方法。 - 請求項4又は5に記載された方法を用いて、前記多結晶SiC成形体を製造する工程と、
前記多結晶SiC成形体を電極として用いて、プラズマエッチングを行う工程と、
を備える、プラズマエッチング方法。
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EP4424870A1 (en) | 2024-09-04 |
KR20240099106A (ko) | 2024-06-28 |
JPWO2023074219A1 (ja) | 2023-05-04 |
JP7374351B2 (ja) | 2023-11-06 |
US20240055236A1 (en) | 2024-02-15 |
CN116670328A (zh) | 2023-08-29 |
TW202328029A (zh) | 2023-07-16 |
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