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WO2021117498A1 - Élément de graphite revêtu de carbonate de tantale et son procédé de production - Google Patents

Élément de graphite revêtu de carbonate de tantale et son procédé de production Download PDF

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Publication number
WO2021117498A1
WO2021117498A1 PCT/JP2020/044124 JP2020044124W WO2021117498A1 WO 2021117498 A1 WO2021117498 A1 WO 2021117498A1 JP 2020044124 W JP2020044124 W JP 2020044124W WO 2021117498 A1 WO2021117498 A1 WO 2021117498A1
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film
tantalum carbide
graphite
coated
reactor
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Japanese (ja)
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狩野　正樹
暁大 平手
山村　和市
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Shin Etsu Chemical Co Ltd
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Shin Etsu Chemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/52—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 carbon, e.g. graphite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • 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
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping

Definitions

  • the present invention relates to a tantalum carbide-coated graphite member used in a semiconductor manufacturing process or the like and a method for manufacturing the same.
  • the graphite member coated with tantalum carbide has excellent heat resistance and chemical stability, it is used as a heat resistant jig especially in a process in which graphite is severely corroded by a reducing gas or a reactive gas.
  • the applicable range of the graphite member coated with TaC is wide, for example, a wafer tray used in a semiconductor manufacturing process. It is used as a raw material melting crucible, a heating source, a reaction vessel, a heat shield member, a crucible for pulling a single crystal, and the like.
  • Known methods for coating TaC on a graphite substrate include an arc ion plating (AIP) type reactive vapor deposition method, a reactive PVD method, and a chemical vapor deposition method (CVD method).
  • AIP arc ion plating
  • PVD reactive PVD
  • CVD chemical vapor deposition method
  • the TaC coating film obtained by these methods has a problem that the film is likely to be peeled off due to the difference in the coefficient of thermal expansion from that of the graphite base material.
  • the TaC film is a hard and brittle material, there is also a problem that cracks are likely to occur due to thermal stress in the film. For example, when used in a high-temperature reducing gas atmosphere, minute cracks may occur and peeling may occur between the graphite base material and the TaC film in about several tens of hours.
  • Patent Document 1 attempts to delay the progress of cracks by forming the TaC film into a crystal structure in which fine particles are densely laminated.
  • the ratio of the peak intensity I (200) of the (200) plane and the peak intensity I (111) of the (111) plane of the X-ray diffraction of the crystal of the TaC layer is set to I (200) / I.
  • (111) 0.2 to 0.5
  • the tantalum carbide-coated graphite member When the tantalum carbide-coated graphite member is used in a reducing gas atmosphere, if the TaC film is thin, the reducing gas permeates the TaC film and reaches the graphite base material, reduces the graphite, and corrodes the graphite. I will go. In this portion, the TaC film is separated from the graphite base material, and the expansion of such a region causes peeling of the graphite base material and the TaC film.
  • an object of the present invention is to provide a tantalum carbide-coated graphite member that is difficult to peel off when used in a high-temperature reducing atmosphere and a method for producing the same.
  • the tantalum carbide-coated graphite member according to the embodiment of the present invention is a tantalum carbide-coated graphite member in which a graphite base material is coated with a tantalum carbide film, and the graphite base material and tantalum carbide are used. It is characterized in that a thermally decomposed boron nitride film is formed between the film and the film.
  • an intermediate layer is formed between the tantalum carbide film and the pyrolysis boron nitride film.
  • an intermediate layer may be formed between the graphite base material and the thermally decomposed boron nitride film.
  • the film thickness of the tantalum carbide film is preferably 0.5 ⁇ m or more and 100 ⁇ m or less.
  • the bulk density of the graphite base material is preferably 1.6 g / cm 3 or more and 2.0 g / cm 3 or less.
  • the film thickness of the pyrolysis boron nitride film is preferably 10 ⁇ m or more and 1000 ⁇ m or less.
  • the method for producing a tantalum carbide-coated graphite member according to the embodiment of the present invention is a step of forming a pyrolysis boron nitride film on a graphite substrate in a first reactor, a step of forming a pyrolysis boron nitride film.
  • the tantalum carbide-coated graphite member according to any one of the above [1] to [6] is produced by the method for producing the tantalum carbide-coated graphite member.
  • a step of forming a pyrolysis boron nitride film on a graphite base material and a step of forming a pyrolysis boron nitride film are coated.
  • the step of coating the tantalum carbide film on the graphite substrate is continuously performed in the same reactor.
  • the tantalum carbide-coated graphite member according to any one of the above [1] to [6] is produced by the method for producing the tantalum carbide-coated graphite member.
  • the tantalum carbide film after treating the surface roughness Rmax of the thermally decomposed boron nitride film to 10 ⁇ m or more.
  • FIG. 1 It is a flowchart which shows the procedure of the manufacturing method of the tantalum carbide coated graphite member. It is sectional drawing of the wafer tray manufactured using the tantalum carbide coated graphite member. It is a front schematic view of the heater manufactured using the tantalum carbide coated graphite member. It is sectional drawing of the heater manufactured using the tantalum carbide coated graphite member in Example 3. FIG. It is sectional drawing of the wafer tray produced using the tantalum carbide coated graphite member in Example 6.
  • FIG. 1 is a flowchart showing a procedure of a method for manufacturing a tantalum carbide-coated graphite member.
  • a graphite base material is prepared (step S10).
  • the graphite base material is processed into an arbitrary shape according to the application by processing means such as machining. If the graphite material used as the base material has a coefficient of thermal expansion close to the coefficient of thermal expansion in the growth plane direction of the pyrolysis boron nitride (PBN) film to be formed later, the thermal stress between the base material and the film is small. It is preferable because it becomes.
  • Anisotropic graphite having an anisotropic coefficient of thermal expansion may be used, but graphite having a ratio of the maximum value to the minimum value of the coefficient of thermal expansion of 1 or more and 1.5 or less is further used. preferable. It is more preferable to use isotropic graphite.
  • the bulk density of the graphite base material is 1.6 g / cm 3 or more, the strength is increased and it is difficult to break, which is preferable.
  • the production of a graphite base material having a bulk density of more than 2.0 g / cm 3 tends to be expensive due to high technical difficulty, and it is preferably 2.0 g / cm 3 or less in consideration of cost performance. ..
  • a pyrolysis boron nitride (PBN) film is formed on the surface of the graphite substrate (step S20).
  • the method for forming the PBN film is not particularly limited, but for example, it can be formed by reacting ammonia (NH 3 ) and boron trichloride (BCl 3 ) at a high temperature of about 1900 ° C. using a CVD method. ..
  • a CVD method there is an advantage that a PBN film having a uniform thickness can be easily formed according to the complicated shape of the base material, and the film quality can be easily densified and highly purified.
  • the film thickness of the PBN film is 10 ⁇ m or more because the effect of preventing the reducing gas from permeating and reaching the graphite base material is further enhanced, and more preferably 30 ⁇ m or more.
  • the film thickness of the PBN film is 10 ⁇ m or more because the effect of preventing the reducing gas from permeating and reaching the graphite base material is further enhanced, and more preferably 30 ⁇ m or more.
  • it is 1000 ⁇ m or less, delamination in the PBN film due to thermal expansion and peeling at the interface between the base material and the PBN film are less likely to occur, and when it is 500 ⁇ m or less, it is more preferable.
  • the PBN film may be formed directly on the graphite base material, but an intermediate layer may be present between the graphite base material and the PBN film.
  • the material of the intermediate layer include pyrolytic graphite, carbon-added pyrolytic graphite, boron carbide, boron-doped pyrolysis graphite (BPG), and the like.
  • BPG boron-doped pyrolytic graphite
  • a graphite base material is placed in a reactor of a CVD device, evacuated, and heated to about 1600 ° C., while methane gas (CH4) and a small amount of boron trichloride are contained in the reactor. It can be formed by supplying (BCl3) and reacting it.
  • a tantalum carbide (TaC) film is formed on the surface of the PBN film (step S30).
  • the method for forming the TaC film is not particularly limited, but it is preferable to use the CVD method.
  • a compound containing a carbon atom such as methane (CH 4 ) and tantalum halide are heated and vaporized and supplied as a raw material, and TaC is reacted at a high temperature of about 900 ° C. to about 1200 ° C. A film can be formed.
  • the CVD method there is an advantage that a TaC film having a uniform thickness can be easily formed according to the complicated shape of the base material, and the film quality can be easily densified and highly purified.
  • the graphite member after forming the PBN film can be moved in a vacuum from the PBN film forming chamber partitioned by a gate valve or the like to the TaC film forming chamber. It is good to say.
  • This closed system is a space that surrounds the members to prevent the inflow of dirty outside air, and keeps the space clean by creating a vacuum or filling the space with clean gas from which dust particles have been removed. Dripping.
  • the surface of the PBN film Before holding the member in the closed system, the surface of the PBN film may be cleaned by acid cleaning, pure water ultrasonic cleaning, or the like, or a part of the surface of the PBN may be ground to make the surface a clean PBN surface. ..
  • the formation of the PBN film and the formation of the TaC film are performed in the film formation chamber of the same apparatus, the apparatus temperature is changed to the temperature of the TaC film formation following the formation of the PBN film, and the reaction gas to be supplied is replaced with the TaC film.
  • the formation may be performed. In this way, it is not necessary to lower the device temperature to room temperature once, which is advantageous in terms of cost.
  • the TaC film may be formed directly on the PBN film, but an intermediate layer may be provided between the PBN film and the TaC film. This is preferable because the adhesion of the TaC film can be further enhanced.
  • the material of the intermediate layer for example, graphite (C), boron-doped graphite, the material of the intermediate composition of PBN and TaC (B x N x Ta z C) , and the like. If the intermediate layer using the B x N y Ta z C further when the gradient composition gradually changes to TaC rich composition from BN rich composition toward the PBN layer side TaC film side preferred.
  • the intermediate layer it is preferable to prevent metal impurities from being mixed into the interface between the PBN film and the intermediate layer.
  • the gas supplied to the reactor should be switched to the raw material gas for forming the intermediate layer to form the intermediate layer.
  • an inclined layer containing a trace amount (about 1% by weight) of carbon may be provided between the PBN film and the intermediate layer.
  • Such an inclined layer can be formed by forming a PBN film while adding a trace amount of methane (CH4) gas, following the formation of a normal PBN film.
  • the gas supplied to the reactor may be further switched to the TaC raw material gas to form the TaC film.
  • the intermediate layer when employing the B x N y Ta z C graded composition as the material of the intermediate layer, when forming the intermediate layer, by passing both the PBN material gas and TaC raw material gas, PBN on the PBN film A film having an intermediate composition between and TaC may be formed, and the PBN raw material gas may be gradually reduced to shift to TaC film formation using only the TaC raw material gas.
  • the film thickness of the TaC film is preferably 0.5 ⁇ m or more and 100 ⁇ m or less, and more preferably 1 ⁇ m or more and 40 ⁇ m or less. If the TaC film is too thick, the internal thermal stress in the TaC film becomes large, and peeling easily occurs at the interface with the PBN film. Further, since the TaC film has a slow growth rate, increasing the film thickness of the TaC film leads to an increase in cost.
  • the growth rate of the PBN film is relatively fast. Therefore, if the PBN film is made thicker than the TaC film, it is advantageous in terms of cost.
  • the TaC film is preferably formed directly on the surface of the PBN film, but an intervening layer may be present between the PBN film and the TaC film.
  • the tantalum carbide-coated graphite member of the present invention exhibits excellent resistance even in an HCl dry etching process under high temperature in a semiconductor manufacturing apparatus, and is used in a semiconductor manufacturing process such as a wafer tray, a raw material melting crucible, a heating source, and a reaction vessel. It can be preferably applied to members requiring heat resistance and corrosion resistance such as heat shield members and crucibles for pulling single crystals.
  • tantalum carbide-coated graphite member of the present invention can be used in a process that dislikes contamination by boron, such as in a Si semiconductor device manufacturing apparatus.
  • FIG. 2 is a schematic cross-sectional view of a wafer tray 1 manufactured using the tantalum carbide-coated graphite member according to Example 1.
  • the wafer tray 1 in Example 1 was produced by the following procedure. First, isotropic graphite was machined to prepare a 100 mm ⁇ 100 mm ⁇ 10 mm graphite base material 2. As shown in FIG. 2, a recess of ⁇ 76 mm is formed on one end surface of the graphite base material 2, and the corner portion is chamfered in an R shape.
  • the graphite base material 2 was placed in the reactor of the CVD apparatus, and the inside of the reactor was evacuated using a vacuum pump and heated to 1900 ° C. Then, ammonia (NH 3 ) and boron trichloride (BCl 3 ) were supplied into the reactor and reacted to form a pyrolysis boron nitride (PBN) film 3 on the surface of the graphite base material 2.
  • the film thickness of the PBN film 3 was set to 300 ⁇ m.
  • tantalum carbide (TaC) film 4 was formed on the surface of the PBN film 3 by supplying methane (CH 4 ) gas and tantalum chloride (TaCl 5) into the reactor and reacting them.
  • the film thickness of the TaC film 4 was 5 ⁇ m.
  • the inside of the reactor was replaced with N 2 , the temperature was lowered to room temperature, and then the reactor was taken out to complete the wafer tray 1 made of tantalum carbide-coated graphite member. No peeling was observed on this wafer tray 1.
  • a thermal shock test was performed on the produced wafer tray 1.
  • the wafer tray 1 was installed in the evaluation device, and the inside of the device was evacuated. Then, it was rapidly heated to 1500 ° C. in about 3 minutes while flowing ammonia (NH 3 ), and the temperature of 1500 ° C. was maintained for 10 minutes. Subsequently, the rapid ascending / descending temperature cycle of cooling to 200 ° C., heating to 1500 ° C. again, and holding for 10 minutes was repeated. The peeling state of the wafer tray 1 was confirmed every cycle.
  • NH 3 ammonia
  • FIG. 3 is a front schematic view of a heater 5 manufactured by using a tantalum carbide-coated graphite member.
  • the heater 5 was manufactured by the following procedure. First, isotropic graphite was machined to prepare a concentric graphite base material having an outer diameter of ⁇ 300 mm, an inner diameter of ⁇ 250 mm, and a thickness of 10 mm.
  • This graphite substrate was placed in the reactor of the CVD apparatus, and the inside of the reactor was evacuated using a vacuum pump and heated to 1900 ° C. Then, ammonia (NH 3 ) and boron trichloride (BCl 3 ) were supplied into the reactor and reacted to form a pyrolysis boron nitride (PBN) film on the surface of the graphite substrate.
  • the film thickness of this PBN film was 10 ⁇ m.
  • tantalum carbide (TaC) film was formed on the surface of the PBN film by supplying methane (CH 4 ) gas and tantalum chloride (TaCl 5) into the reactor and reacting them.
  • the film thickness of this TaC film was 1 ⁇ m.
  • the produced heater 5 was energized and heated. First, the heater 5 was installed in the evaluation device, and the inside of the device was evacuated. Then, electricity was applied while flowing ammonia (NH 3 ), the mixture was heated to 1500 ° C. in about 30 minutes, and the temperature of 1500 ° C. was maintained for 10 minutes. Subsequently, the rapid ascending / descending temperature cycle of cooling to 200 ° C., heating to 1500 ° C. again and holding for 10 minutes was repeated. The peeling state was confirmed every cycle.
  • NH 3 ammonia
  • FIG. 4 is a schematic cross-sectional view of the heater 5A manufactured by using the tantalum carbide-coated graphite member according to the third embodiment.
  • the heater 5A in Example 3 was produced by the following procedure. First, isotropic graphite was machined to prepare a graphite base material 2A having the same shape as in Example 2.
  • the graphite base material 2A was placed in the reactor of the CVD apparatus, and the inside of the reactor was evacuated using a vacuum pump and heated to 1900 ° C. Then, ammonia (NH 3 ) and boron trichloride (BCl 3 ) were supplied into the reactor and reacted to form a pyrolysis boron nitride (PBN) film 3A on the surface of the graphite base material 2A.
  • the film thickness of the PBN film 3A was set to 50 ⁇ m, and a small amount of methane (CH 4 ) gas was further added to provide an inclined layer 6A having a thickness of about 1 to 2 ⁇ m so that the carbon concentration in the PBN was about 1% by weight.
  • the inside of the reactor was evacuated with the base material 2 on which the PBN film 3A was formed contained in the reactor, and the temperature inside the reactor was set to 1600 ° C. Then, by supplying methane (CH 4 ) gas and a small amount of BCl 3 gas into the reactor and reacting them, a boron-doped graphite film to be an intermediate layer 7A was formed on the surface of the PBN film 3A. The film thickness of this boron-doped graphite film was 2 ⁇ m. The boron concentration in the pyrolytic carbon at this time was 6 to 8% by weight.
  • the inside of the reactor was put into a vacuum state, the temperature inside the reactor was set to 1500 ° C., and heat treatment was performed for 1 hour. Then, by supplying methane (CH 4 ) gas and tantalum chloride (TaCl 5 ) into the reactor and reacting them, a tantalum carbide (TaC) film 4A is formed on the surface of the PBN film 3A with the intermediate layer 7A sandwiched between them. did.
  • the film thickness of the TaC film 4A was set to 5 ⁇ m.
  • the base material 2A was taken out from the reactor to complete the heater 5A of the tantalum carbide-coated graphite member. No peeling was observed in this heater 5A.
  • the produced heater 5A was energized and heated. First, the heater 5A was installed in the evaluation device, and the inside of the device was evacuated. Then, electricity was applied while flowing ammonia (NH 3 ), the mixture was heated to 1500 ° C. in about 30 minutes, and the temperature of 1500 ° C. was maintained for 10 minutes. Subsequently, the rapid ascending / descending temperature cycle of cooling to 200 ° C., heating to 1500 ° C. again, and holding for 10 minutes was repeated. The peeling state was confirmed every cycle.
  • NH 3 ammonia
  • Example 4 First, isotropic graphite was machined to prepare a graphite substrate having the same shape as in Example 2.
  • This graphite substrate was placed in the reactor of the CVD apparatus, and the inside of the reactor was evacuated using a vacuum pump and heated to 1900 ° C. Then, ammonia (NH 3 ) and boron trichloride (BCl 3 ) were supplied into the reactor and reacted to form a pyrolysis boron nitride (PBN) film on the surface of the graphite substrate.
  • the film thickness of this PBN film was 50 ⁇ m.
  • the graphite base material on which the PBN film was formed was once taken out from the reactor, the surface was washed with pure water, and the mixture was placed in a CVD reactor.
  • a clean dry N 2 (dew point ⁇ 75 ° C.) was poured into the anti-container at normal pressure to 1600 ° C. for 30 minutes, and then the inside of the anti-container was evacuated and held for 30 minutes.
  • methane (CH 4 ) gas and tantalum chloride (TaCl 5 ) were supplied to the reactor and reacted to form a tantalum carbide (TaC) film on the surface of the PBN film.
  • the film thickness of this TaC film was 5 ⁇ m.
  • Example 5 First, isotropic graphite was machined to prepare a graphite substrate having the same shape as in Example 2.
  • This graphite substrate was placed in the reactor of the CVD apparatus, and the inside of the reactor was evacuated using a vacuum pump and heated to 1900 ° C. Then, ammonia (NH 3 ) and boron trichloride (BCl 3 ) were supplied into the reactor and reacted to form a pyrolysis boron nitride (PBN) film on the surface of the graphite substrate.
  • the film thickness of this PBN film was 55 ⁇ m.
  • the graphite base material on which the PBN film was formed was once taken out from the reactor, and the surface was ground to obtain a surface roughness Rmax of 12 ⁇ m. After that, the ground surface was washed with aqua regia, then ultrasonically washed with pure water, dried by heating at 120 ° C., and placed in a CVD reactor. The inside of the reactor was evacuated, heated to 120 ° C., and held for 30 minutes. Then, methane (CH 4 ) gas and tantalum chloride (TaCl 5 ) were supplied to the reactor and reacted to form a tantalum carbide (TaC) film on the surface of the PBN film. The film thickness of this TaC film was 5 ⁇ m.
  • the temperature was lowered to room temperature, and then taken out to complete the heater 5 of the tantalum carbide-coated graphite member. No peeling was observed in this heater 5.
  • the produced heater 5 was energized and heated. First, the heater 5 was installed in the evaluation device, and the inside of the device was evacuated. Then, electricity was applied while flowing ammonia (NH 3 ), the mixture was heated to 1500 ° C. in about 30 minutes, and the temperature of 1500 ° C. was maintained for 10 minutes. Subsequently, the rapid ascending / descending temperature cycle of cooling to 200 ° C., heating to 1500 ° C. again, and holding for 10 minutes was repeated. The peeling state was confirmed every cycle.
  • NH 3 ammonia
  • FIG. 5 is a schematic cross-sectional view of a wafer tray 1B manufactured by using the tantalum carbide-coated graphite member according to Example 6.
  • the wafer tray 1B in Example 6 was produced by the following procedure. First, isotropic graphite was machined to prepare a graphite base material 2B of a wafer tray similar to that in Example 1.
  • This graphite base material 2B was placed in the reactor of the CVD apparatus, and the inside of the reactor was evacuated using a vacuum pump and heated to 1600 ° C.
  • a boron-doped pyrolytic graphite (BPG) film is formed as an intermediate layer 7B on the surface of the graphite base material 2B. 2 ⁇ m was formed.
  • the inside of the reactor is heated to 1850 ° C., and ammonia (NH 3 ) and boron trichloride (BCl 3 ) are supplied into the reactor to react, thereby intermediate between BPG.
  • a pyrolysis boron nitride (PBN) film 3B of 75 ⁇ m was formed on the surface of the layer 7B.
  • a small amount of methane gas (CH 4 ) was flowed to further form an intermediate layer 8B of 3 ⁇ m carbon-doped pyrolysis boron nitride (PBCN).
  • tantalum carbide (TaC) film 4B was formed on the surface of the PBN film provided with the intermediate layer 8B.
  • the temperature was lowered to room temperature, and then the reactor was taken out to complete the wafer tray 1B of the tantalum carbide-coated graphite member. No peeling was observed in this wafer tray 1B.
  • a thermal shock test was performed on the produced wafer tray 1B.
  • the wafer tray 1B was installed in the evaluation device, and the inside of the device was evacuated. Then, it was rapidly heated to 1500 ° C. in about 3 minutes while flowing ammonia (NH 3 ), and the temperature of 1500 ° C. was maintained for 10 minutes. Subsequently, the rapid ascending / descending temperature cycle of cooling to 200 ° C., heating to 1500 ° C. again and holding for 10 minutes was repeated. The peeling state of the wafer tray 1B was confirmed every cycle.
  • NH 3 ammonia
  • Isotropic graphite was machined to prepare a 100 mm ⁇ 100 mm ⁇ 10 mm graphite substrate.
  • a recess of ⁇ 76 mm is formed on one end surface of the graphite base material, and the corners are chamfered in an R shape.
  • This graphite substrate was placed in the reactor of the CVD apparatus, the inside of the reactor was evacuated using a vacuum pump, and the mixture was heated to 900 ° C. Then, tantalum carbide (TaC) film was formed on the surface of the PBN film by supplying methane (CH 4 ) gas and tantalum chloride (TaCl 5) into the reactor and reacting them. The film thickness of this TaC film was 5 ⁇ m.
  • a thermal shock test was performed on the produced wafer tray. First, the wafer tray was installed in the evaluation device, and the inside of the device was evacuated. Then, it was rapidly heated to 1500 ° C. in about 3 minutes while flowing ammonia (NH 3 ), and the temperature of 1500 ° C. was maintained for 10 minutes. Subsequently, the rapid ascending / descending temperature cycle of cooling to 200 ° C., heating to 1500 ° C. again, and holding for 10 minutes was repeated. The peeling state was confirmed every cycle.
  • NH 3 ammonia
  • the manufactured wafer tray had cracks at the corners and peeling occurred when the rapid temperature raising / lowering cycle was repeated 50 times.
  • ⁇ Comparative example 2> A wafer tray made of tantalum carbide-coated graphite member was completed in the same manner as in Comparative Example 1. However, in Comparative Example 2, the film thickness of the TaC film was set to 50 ⁇ m.
  • a tantalum carbide-coated graphite member that does not easily peel off the coating film even when used in a high-temperature reducing atmosphere can be obtained. be able to.

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  • Chemical Vapour Deposition (AREA)

Abstract

La présente invention concerne un élément de graphite revêtu de carbonate de tantale difficile à décoller durant l'utilisation sous une atmosphère réductrice à haute température, et son procédé de production. L'élément de graphite revêtu de carbonate de tantale selon la présente invention comprend un matériau à base de graphite revêtu d'un film de carbonate de tantale, caractérisé en ce qu'un film de nitrure de bore pyrolytique est formé entre le matériau à base de graphite et le film de carbonate de tantale. Le procédé de production de l'élément de graphite revêtu de carbonate de tantale est caractérisé en ce qu'une étape de revêtement d'un matériau à base de graphite avec un film de nitrure de bore pyrolytique et qu'une étape de revêtement du matériau à base de graphite revêtu du film de nitrure de bore pyrolytique avec un film de carbonate de tantale sont successivement effectuées dans un réacteur unique.
PCT/JP2020/044124 2019-12-12 2020-11-26 Élément de graphite revêtu de carbonate de tantale et son procédé de production Ceased WO2021117498A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114368984A (zh) * 2022-01-27 2022-04-19 中电化合物半导体有限公司 一种碳基体的涂层及其制备方法与应用
WO2024143947A1 (fr) * 2022-12-29 2024-07-04 주식회사 티씨케이 Matériau revêtu de carbure de tantale

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Publication number Priority date Publication date Assignee Title
JPH10506677A (ja) * 1994-09-28 1998-06-30 アドヴァンスト・セラミックス・コーポレイション 多層フラッシュエバポレーター
JP2007016272A (ja) * 2005-07-06 2007-01-25 Ge Speciality Materials Japan Kk 基板上に被覆形成される保護膜及びその製造方法
WO2010122801A1 (fr) * 2009-04-24 2010-10-28 独立行政法人産業技術総合研究所 Appareil concu pour fabriquer un monocristal de nitrure d'aluminium, procede de fabrication du monocristal de nitrure d'aluminium, et monocristal de nitrure d'aluminium
JP2015193872A (ja) * 2014-03-31 2015-11-05 トーカロ株式会社 セラミック溶射皮膜被覆部材及び半導体製造装置用部材

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10506677A (ja) * 1994-09-28 1998-06-30 アドヴァンスト・セラミックス・コーポレイション 多層フラッシュエバポレーター
JP2007016272A (ja) * 2005-07-06 2007-01-25 Ge Speciality Materials Japan Kk 基板上に被覆形成される保護膜及びその製造方法
WO2010122801A1 (fr) * 2009-04-24 2010-10-28 独立行政法人産業技術総合研究所 Appareil concu pour fabriquer un monocristal de nitrure d'aluminium, procede de fabrication du monocristal de nitrure d'aluminium, et monocristal de nitrure d'aluminium
JP2015193872A (ja) * 2014-03-31 2015-11-05 トーカロ株式会社 セラミック溶射皮膜被覆部材及び半導体製造装置用部材

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114368984A (zh) * 2022-01-27 2022-04-19 中电化合物半导体有限公司 一种碳基体的涂层及其制备方法与应用
WO2024143947A1 (fr) * 2022-12-29 2024-07-04 주식회사 티씨케이 Matériau revêtu de carbure de tantale

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