JP2019099453A - Tantalum carbide coating carbon material and method of manufacturing the same, and member for semiconductor single-crystal manufacturing apparatus - Google Patents

Abstract

To provide a member for semiconductor single-crystal manufacturing apparatus which has a long product lifetime, and a tantalum carbide coating carbon material.SOLUTION: A tantalum carbide coating carbon material according to the present invention is characterized in that: at least a part of a carbon base material surface is coated with a tantalum carbide coating film consisting principally of tantalum carbide; and the tantalum carbide coating film has an intensity of X-ray diffracted rays, corresponding to a (200) plane in a plane outward direction larger than intensities of X-ray diffracted rays corresponding to other crystal planes; and the intensity ratio thereof is 60% or larger of the sum of intensities of X-ray diffracted rays corresponding to the entire crystal plane.SELECTED DRAWING: Figure 4

Description

  The present invention relates to a tantalum carbide-coated carbon material in which a tantalum carbide film is coated on the surface of a carbon substrate, and a member for a semiconductor single crystal production apparatus using this material.

  Tantalum carbide has the highest melting point (about 3900 ° C.) among transition metal carbides, and is also excellent in chemical stability, strength, toughness, and corrosion resistance. Therefore, a tantalum carbide-coated carbon material in which a tantalum carbide film is coated on the surface of a carbon substrate is used as a member in a semiconductor single crystal manufacturing apparatus such as Si (silicon), SiC (silicon carbide), GaN (gallium nitride) There is.

  A sublimation recrystallization method (modified Lely method) is widely known as a method of producing a bulk single crystal of SiC. In the sublimation recrystallization method, the inside of a crucible is filled with a SiC raw material, and a SiC seed crystal is disposed on the upper part thereof. In addition, a cylindrical guide member is installed around the SiC seed crystal. The sublimation gas generated by the heating of the SiC raw material rises along the inner wall of the guide member, and the SiC single crystal grows with the SiC seed crystal.

  In addition, a SiC single crystal substrate used for semiconductor devices and the like is manufactured by epitaxially growing a SiC single crystal on a bulk single crystal SiC substrate. As a method of epitaxially growing a SiC single crystal, a liquid phase epitaxy (LPE) method, a vapor phase epitaxy (VPE) method, a chemical vapor deposition (CVD) method and the like are known. In general, the method of epitaxially growing a SiC single crystal is the CVD method. In the epitaxial growth method by the CVD method, the SiC substrate is mounted on a susceptor in the apparatus, and the raw material gas is supplied at a high temperature of 1500 ° C. or more to grow the SiC single crystal.

  In such a method of producing a SiC single crystal, in order to obtain higher quality crystals, Patent Document 1 discloses a method of using a crucible in which the inner surface of a graphite base is coated with tantalum carbide. Further, Patent Document 2 discloses a method using a guide member whose inner wall is coated with tantalum carbide.

  In addition, the tantalum carbide-coated film in the tantalum carbide-coated carbon material is attempted to improve the characteristics by controlling its orientation. For example, in Patent Document 3, the corrosion resistance and the thermal shock resistance are improved by specifically developing the (220) plane of tantalum carbide with respect to other crystal planes.

Unexamined-Japanese-Patent No. 11-116398 JP 2005-225710 A JP 2008-308701 A

  It is known that metal carbides differ in chemical activity (reactivity) depending on their crystal faces. The reactivity is considered to be high on the (111) plane, the (220) plane, the (311) plane, and the (222) plane of tantalum carbide because the atomic densities of tantalum (Ta) and carbon (C) are not equal.

  Therefore, when the tantalum carbide-coated carbon material as shown in Patent Document 3 is used as a member for a semiconductor single crystal production apparatus, the product life is shortened because the reactivity of the tantalum carbide coating film is high. I am concerned.

  Then, an object of this invention is to provide the member for semiconductor single crystal manufacturing apparatuses with a long product life, and a tantalum carbide covering carbon material.

  In order to solve the above problems, the tantalum carbide-coated carbon material according to the present invention is a tantalum carbide-coated carbon material in which at least a part of the surface of a carbon substrate is coated with a tantalum carbide coating film containing tantalum carbide as a main component. . In this tantalum carbide-coated carbon material, the intensity of the X-ray diffraction line corresponding to the (200) plane in the out-of-plane direction is greater than the intensity of the X-ray diffraction line corresponding to the other crystal planes It is characterized by being 60% or more with respect to the sum of the intensities of the X-ray diffraction lines corresponding to the surface.

  According to such a configuration, the product life of the tantalum carbide-coated carbon material can be extended.

  In the tantalum carbide coated carbon material according to the present invention, the arithmetic average roughness Ra of the surface of the tantalum carbide coating film may be 3.5 μm or less.

  In the tantalum carbide coated carbon material according to the present invention, the arithmetic mean roughness Ra of the surface of the carbon substrate may be 4.0 μm or less.

  In the tantalum carbide-coated carbon material according to the present invention, the number of tantalum atoms contained in the tantalum carbide coating film may be greater than the number of carbon atoms and 1.2 times or less the number of carbon atoms.

  In the tantalum carbide coated carbon material according to the present invention, the tantalum carbide coating film preferably contains chlorine atoms at an atomic concentration of 0.01 atm% or more and 1.00 atm% or less.

  The member for a semiconductor single crystal production device according to the present invention is made of a tantalum carbide coated carbon material. This member for manufacturing a semiconductor single crystal is a member in which at least a part of the surface of the carbon base material is covered with a tantalum carbide coating film mainly composed of tantalum carbide, and corresponds to the (200) plane in the out-of-plane direction The intensity of the X-ray diffraction line is greater than the intensity of X-ray diffraction lines corresponding to other crystal planes, and the intensity ratio is 60% or more with respect to the sum of the intensities of X-ray diffraction lines corresponding to all crystal planes It is characterized by being.

  According to such a configuration, it is possible to prolong the product life of the member for a semiconductor single crystal manufacturing device configured from the tantalum carbide coated carbon material. As a result, the manufacturing cost of the semiconductor single crystal can be reduced.

  The member for a semiconductor single crystal manufacturing apparatus according to the present invention may be used in a manufacturing apparatus of a SiC single crystal.

  The member for a semiconductor single crystal production apparatus according to the present invention is preferably a crucible or a guide member used in an apparatus for producing a SiC single crystal by a sublimation recrystallization method.

  The member for a semiconductor single crystal production apparatus according to the present invention may be a susceptor or an inner wall member used for a device for epitaxially growing a SiC single crystal by a chemical vapor deposition method.

  The member for a semiconductor single crystal production device according to the present invention may have two or more locations with a low tantalum atom concentration on the surface of the tantalum carbide coating film.

  The method for producing a tantalum carbide-coated carbon material according to the present invention comprises the steps of preparing a carbon substrate having an arithmetic surface roughness Ra of 4.0 μm or less, and at least a part of the surface of the carbon substrate with a tantalum carbide coating film. And covering the

  According to such a configuration, the strength ratio of the X-ray diffraction line corresponding to the peeling strength between the carbon base material and the tantalum carbide coating film of 1 MPa or more and the (200) plane of the tantalum carbide coating film is the entire A tantalum carbide coated carbon material can be produced with features that are at least 60% of the intensity sum of the x-ray diffraction lines.

  In the method for producing a tantalum carbide-coated carbon material according to the present invention, the preparing step includes a step of supporting a carbon substrate in a reaction chamber, and the coating step is a raw material including a compound containing carbon atoms and tantalum halide. It is preferable to have the steps of: supplying a gas into the reaction chamber; and reacting the supplied source gas by a thermal CVD method to form a tantalum carbide coated film.

  In the method for producing a tantalum carbide-coated carbon material according to the present invention, the carbon substrate may be coated with a tantalum carbide coating while rotating about a rotation axis. In this method, the rotation axis may be coated with the tantalum carbide film while revolving around the revolution axis.

  In the method for producing a tantalum carbide-coated carbon material according to the present invention, the temperature in the reaction chamber may be set to 850 ° C. or more and 1200 ° C. or less in the step of supplying the source gas.

In the method for producing a tantalum carbide-coated carbon material according to the present invention, in the step of supplying the raw material gas, the compound containing carbon atoms is preferably methane (CH ₄ ), and the halogenated tantalum is tantalum pentachloride (TaCl ₅ ). Good. The flow ratio of methane and tantalum pentachloride to be supplied may be 2 or more and 20 or less.

  The method for producing a tantalum carbide-coated carbon material according to the present invention may further include a step of annealing the carbon substrate on which the tantalum carbide coating film is formed after the step of coating.

FIG. 1 shows a schematic view of an external heating type low pressure CVD apparatus 1; The schematic of the pressure-reduction heating furnace 8 for making a SiC single crystal grow by the sublimation recrystallization method is shown. FIG. 1 shows a schematic view of a CVD apparatus 1 for epitaxially growing a SiC single crystal. 1 shows the XRD pattern of the tantalum carbide coated film of Example 1. FIG. 18 shows an XRD pattern of the tantalum carbide coated film of Example 3. The XRD pattern of the tantalum carbide coating film of the comparative example 1 is shown. The XRD pattern of the tantalum carbide coating film of the comparative example 3 is shown. The XRD pattern of the tantalum carbide coating film of the comparative example 4 is shown. It is the schematic which shows the structure of an external heating type | mold low pressure CVD apparatus which forms a tantalum carbide coating film, rotating a carbon base material. FIG. 10A is a schematic view showing the configuration of an external heating type low pressure CVD apparatus for forming a tantalum carbide coating film while rotating and revolving a carbon substrate. FIG. 10 (b) is a plan view showing rotation and revolution.

  Hereinafter, although an embodiment of the present invention is explained in full detail, the present invention is not limited to this.

  The tantalum carbide-coated carbon material of the present invention is composed of a carbon substrate and a tantalum carbide coating film containing tantalum carbide as a main component, and at least a part of the surface of the carbon substrate is coated with the tantalum carbide coating film.

  As the carbon substrate 4, carbon materials such as isotropic graphite, extruded graphite, pyrolytic graphite, and a carbon fiber reinforced carbon composite material (C / C composite) can be used. The shape and characteristics thereof are not particularly limited, and can be processed into any shape according to the application and the like.

  The tantalum carbide coating film containing tantalum carbide as a main component can be formed by a method such as a chemical vapor deposition (CVD) method, a sintering method, and a carbonization method. Among them, the CVD method is preferable as a method for forming a tantalum carbide coating film because a uniform and dense film can be formed.

  Further, the CVD method includes a thermal CVD method, a photo CVD method, a plasma CVD method and the like, and for example, the thermal CVD method can be used. The thermal CVD method has advantages such as relatively simple apparatus configuration and no damage by plasma. The formation of the tantalum carbide coating film by the thermal CVD method can be performed using, for example, an external heating type low pressure CVD apparatus 1 as shown in FIG.

In the external heating type low pressure CVD apparatus 1, the carbon substrate 4 is supported by the support means 5 in the reaction chamber 2 provided with the heater 3, the raw material supply unit 6, the exhaust unit 7 and the like. Then, as a raw material gas, a raw material supply unit 6 supplies a compound containing a carbon atom such as methane (CH ₄ ) and a halogenated tantalum such as tantalum pentachloride (TaCl ₅ ). The halogenated tantalum gas can be generated, for example, by a method of heating and vaporizing a halogenated tantalum, a method of reacting tantalum metal and a halogen gas, or the like. Subsequently, the raw material gas supplied from the raw material supply unit 6 is subjected to a thermal CVD reaction under reduced pressure at a high temperature of 900 to 1200 ° C. and 1 to 100 Pa to form a tantalum carbide coating film on the carbon substrate 4.

  The tantalum carbide coating film contains tantalum carbide as a main component, but may contain a small amount of atoms other than carbon and tantalum. Specifically, the tantalum carbide coating film may contain 1.0 atm% or less of an impurity element or a doping element.

  The tantalum carbide coating film may coat the entire surface of the carbon substrate 4 or may cover only a part of the surface, depending on the use and the form of use. In addition, the tantalum carbide coating film may be formed in plural times and laminated. By changing the portion supporting the carbon substrate 4 in the first and second times to form a film, it is possible to surely eliminate the exposed portion of the carbon substrate 4 and the portion having a low tantalum atom concentration, but the manufacturing cost Will increase.

  When forming a tantalum carbide coating film, the position at which the carbon substrate 4 is mounted is shifted from the center of the heater 3, or the heater 3 is deteriorated with time, and the heat generation distribution in the circumferential direction becomes uneven. As a result, the surface temperature of the carbon substrate 4 may become uneven in the circumferential direction, which may cause uneven film formation. In order to average the distribution of such film formation amount during film formation, the carbon substrate 4 may be coated while rotating about its rotation axis. For example, as shown in FIG. 9, the support means 5 can be rotated about the vertical axis, and the carbon base 4 is supported so that its rotation axis coincides with the rotation axis of the support means 5. Then, a tantalum carbide coating film is formed while rotating the support means 5. In this way, a uniform coating film can be formed in the circumferential direction of the rotation axis of the carbon base 4. The method of coating while rotating in this manner is particularly effective when the shape of the carbon substrate 4 is a rotating body or a rotationally symmetric body. In addition, when the carbon base material 4 is a rotary body or rotational symmetry, it is preferable to arrange | position so that the symmetry axis of the carbon base material 4 and a rotation axis may correspond. Furthermore, the flow of gas in the reaction chamber 2 until it ejects from the raw material supply unit 6 and is discharged by the exhaust unit 7 differs depending on the shape of the carbon substrate 4 and the supporting method. For this reason, the concentration distribution of the film forming substance is generated in the reaction chamber 2, and the film forming target surface of the carbon substrate 4 has a position not to form a film (even if the film forming amount is averaged by rotation). is there. Therefore, the flow of gas relative to the autorotating carbon base material 4 in the reaction chamber 2 is intentionally asymmetric (rotational asymmetry or rotational It may be plane asymmetry. For this purpose, the raw material supply unit 6 and the exhaust unit 7 may be installed at a position shifted from the extension of the rotation axis of the carbon substrate 4, and the gas ejected from the raw material supply unit 6 has an inclination θ with respect to the rotation axis. Alternatively, the angle θ may be adjusted.

  Further, in the configuration in which the carbon base material 4 is coated while rotating around its rotation axis, the coating film may be formed while revolving around the rotation axis of another rotation axis. For example, as shown in FIG. 10 (a), a plurality of support means 5 rotatable around the vertical axis are prepared, and they are arranged to revolve around the common revolution axis, and the carbon base 4 is supported It is supported by the means 5. In this manner, a plurality of carbon substrates 4 rotating on a revolving track are arranged, and as shown in FIG. 10B, a tantalum carbide coating film is formed while rotating each carbon substrate 4 while rotating. In this way, the coating film formed on each carbon substrate can be uniformly aligned. At this time, it is preferable that the rotational speed of the carbon substrate 4 is not an integral multiple of the rotational speed of revolution (for example, 2.1 times, 2.3 times, etc.). In this way, the rotation angle of the carbon substrate 4 (in other words, the position angle of the carbon substrate closest to the heater 3) every time the rotation axis of the carbon substrate 4 revolves once and reaches the same rotation angle position. Can be different. Thereby, it is possible to reduce the unevenness of film formation on the film formation symmetrical surface of the carbon substrate 4. However, even if the rotation speed of the rotation is a non-integral multiple of the rotation speed of revolution, the rotation ratio (for example, 2.5 times) at which the orientation of the carbon substrate 4 deviates by 180 ° once is 2 When it is reciprocated, the orientation of the carbon base material 4 returns to the original position (0 °), and the elliptical shape is easily deviated, so it is preferable to avoid this. For the same reason, it is preferable to avoid a rotational ratio at which the orientation of the carbon substrate 4 deviates by 120 °, 90 °, 72 ° (or 144 °) and 60 ° when reciprocated once. At this time, the flow of the gas to the revolving carbon substrate 4 may be intentionally made asymmetric so that the film-forming substance is completely spread on the film formation symmetry plane of each carbon substrate. For this purpose, the raw material supply unit 6 is offset with respect to the revolution axis to have an offset t, and the offset t is formed so as to form a desired coating film according to the shape of the carbon substrate 4 and the revolution radius. You may adjust the Moreover, you may make it incline with respect to a revolution axis or a rotation axis. When it is desired to apply a coating to only a part of each of the plurality of carbon substrates 4, the carbon substrate 4 can be coated only by revolution without being rotated.

  In the present invention, in the tantalum carbide-coated film, the intensity of the X-ray diffraction line corresponding to the (200) plane in the out-of-plane direction is larger than the intensity of the X-ray diffraction line corresponding to other crystal planes, and the intensity ratio Is 60% or more with respect to the sum of the intensities of X-ray diffraction lines corresponding to all crystal planes.

  The intensity of the X-ray diffraction line of the tantalum carbide coating is obtained by 2θ / θ measurement (out-of-plane) using an X-ray diffractometer (XRD). The peak corresponding to the (200) plane of the tantalum carbide crystal is observed around 2θ = 40 °.

  If the peak intensity corresponding to this (200) plane is larger than the peaks corresponding to other crystal planes, and the intensity ratio is 60% or more with respect to the sum of peak intensities corresponding to all crystal planes, tantalum carbide coating The product life of a member for a semiconductor single crystal production apparatus using a carbon material can be extended. This is considered to be due to the fact that the atomic density of carbon and tantalum is equivalent in the (200) plane of tantalum carbide, and the reactivity on the surface of the tantalum carbide coating becomes low.

The intensity and intensity ratio of the X-ray diffraction line corresponding to the (200) plane of the tantalum carbide coating film are determined by various film forming conditions. When a tantalum carbide coating film is formed using a thermal CVD method, if the reaction temperature in the reaction chamber 2 is set to 1000 ° C. or more and 1200 ° C. or less, the intensity of the X-ray diffraction line corresponding to the (200) plane is It tends to be greater than the intensity of X-ray diffraction lines corresponding to other crystal planes. In addition, by annealing at about 2000-2500 ° C. after film formation, the intensity of the X-ray diffraction line corresponding to the (200) plane tends to be greater than the intensity of the X-ray diffraction line corresponding to other crystal planes. is there. Furthermore, the flow ratio of the source gas (methane and tantalum pentachloride) supplied into the reaction chamber 2 affects the intensity of the X-ray diffraction line corresponding to the (200) plane. For example, when the flow ratio (CH ₄ / TaCl ₅ ) of the source gas supplied into the reaction chamber 2 is 4.0 to 6.0, the intensity of the X-ray diffraction line corresponding to the (200) plane tends to increase. is there.

  The arithmetic mean roughness Ra of the surface of the carbon substrate also affects the intensity and intensity ratio of the X-ray diffraction line corresponding to the (200) plane of the tantalum carbide coating film. The larger the value of the arithmetic mean roughness Ra of the surface of the carbon substrate, the greater the peel strength between the carbon substrate 4 and the tantalum carbide coating film, which is preferable, but on the other hand, the (200) plane There is a tendency that the intensity ratio of the corresponding X-ray diffraction line becomes smaller. Therefore, from the viewpoint of the intensity ratio of X-ray diffraction lines corresponding to the (200) plane, the arithmetic mean roughness Ra of the surface of the carbon substrate is preferably 4.0 μm or less.

  The arithmetic mean roughness of the surface of the carbon substrate 4 is considered in consideration of the peel strength between the carbon substrate 4 and the tantalum carbide coating and the intensity ratio of X-ray diffraction lines corresponding to the (200) plane of the tantalum carbide coating. The thickness Ra is preferably 0.5 μm or more and 4.0 μm or less, and more preferably 1.0 μm or more and 3.0 μm or less. In this way, the peel strength between the carbon substrate 4 and the tantalum carbide coating film is 1 MPa or more, and the intensity ratio of the X-ray diffraction line corresponding to the (200) plane of the tantalum carbide coating film is 60% or more. It is possible to make it easy.

  Furthermore, arithmetic mean roughness Ra of the tantalum carbide coating film surface is preferably 3.5 μm or less, and more preferably 3.0 μm or less. If the value of the arithmetic average roughness Ra on the surface of the tantalum carbide coating film is large, the product life when used as a member for a semiconductor single crystal production apparatus may be shortened. It is considered that this is because the surface area is smaller and the reactivity is lower as the unevenness on the surface of the tantalum carbide coating film is smaller.

  Arithmetic mean roughness Ra of the tantalum carbide coating film surface immediately after film formation fluctuates according to arithmetic mean roughness Ra of the carbon base material surface, is slightly smaller than arithmetic mean roughness Ra of the carbon base material surface Tend. Arithmetic mean roughness Ra of the tantalum carbide coating film surface can be controlled by polishing or the like, but since the number of manufacturing steps is increased, carbon is selected according to the desired arithmetic mean roughness Ra of the tantalum carbide coating film surface. It is preferable to select the arithmetic mean roughness Ra of the surface of the substrate 4.

  As described above, the arithmetic mean roughness Ra of the surface of the carbon base 4 affects the peel strength between the carbon base 4 and the tantalum carbide coating, and it is not preferable that the value is too small. Therefore, the arithmetic average roughness Ra of the tantalum carbide coating film surface is preferably 0.4 μm or more, more preferably 0.8 μm or more, in accordance with the arithmetic average roughness Ra of the surface of the carbon base 4 preferable.

  In addition, arithmetic mean roughness Ra here is the value measured based on JIS B 0633: 2001 (ISO 4288: 1996).

The number of tantalum atoms contained in the tantalum carbide coating film is preferably greater than the number of carbon atoms and not more than 1.2 times the number of carbon atoms, and more preferably 1.05 to 1.15. . That is, it is represented by Ta _x C (1.0 <x ≦ 1.2).

  If the number of carbon atoms is large, many carbon atoms will be present in the tantalum carbide coating. Since carbon has higher reactivity than tantalum, the reactivity of the tantalum carbide coating film is increased, and the product life when used as a member for a semiconductor single crystal production apparatus is shortened. On the other hand, if the number of tantalum atoms is increased, carbon atoms are reduced, the reactivity of the tantalum carbide coating film can be lowered, and the product life when used as a member for a semiconductor single crystal production apparatus is also extended.

  Further, the atomic concentration of chlorine atoms contained in the tantalum carbide coating film is preferably 0.01 atm% or more and 1.00 atm% or less, and more preferably 0.02 atm% or more and 0.06 atm% or less . An excessively high atomic concentration of chlorine atoms is not preferable because it affects the characteristics of the tantalum carbide coating film, but by including an atomic concentration of chlorine atoms to some extent, the concentration of impurity metals such as iron in the coating film is lowered It is possible to

  In the member for a semiconductor single crystal production apparatus of the present invention, at least a part of the surface of the carbon base 4 is made of a tantalum carbide coated carbon material coated with a tantalum carbide coating film containing tantalum carbide as a main component. In this tantalum carbide coating film, the intensity of the X-ray diffraction line corresponding to the (200) plane in the out-of-plane direction is larger than the intensity of the X-ray diffraction line corresponding to other crystal planes, and the intensity ratio is the entire crystal It is 60% or more with respect to the sum of the intensities of the X-ray diffraction lines corresponding to the surface.

  If it is a member for such a semiconductor single crystal manufacturing apparatus, it can suppress that a semiconductor single crystal adheres to a member in the growth process of a semiconductor single crystal, and can extend product life. This is considered to be due to the fact that the atomic density of carbon and tantalum is equal in the (200) plane of tantalum carbide, and the reactivity is lower than in other crystal planes. It is not limited to the type or manufacturing method.

  On the other hand, tantalum carbide is low in wettability to silicon carbide (SiC), and it can be expected to prolong the life of the member. Therefore, conventionally, a tantalum carbide-coated carbon material is used as a member for a SiC single crystal manufacturing apparatus ing. Therefore, susceptor 21 and inner wall member 18 used in an apparatus for epitaxially growing SiC single crystal by CVD method, which is used in an apparatus for producing a SiC single crystal by a sublimation recrystallization method. Especially useful as

  A member for a semiconductor single crystal production apparatus can be obtained, for example, by using a carbon material processed into the shape of the member as the carbon base 4 and covering the surface with a tantalum carbide coating film containing tantalum carbide as a main component. If necessary, further processing may be performed, or other materials may be used in combination.

  When the tantalum carbide coating film is coated on the carbon substrate 4, the method described above can be used, and for example, a thermal CVD method can be used.

  At this time, it is preferable that the support means 5 for supporting the carbon substrate 4 have a support portion with a pointed tip, and the tip of the support portion support the carbon substrate 4 at two or more places. It is more preferable to support at three places. In this way, the contact area between the tip of the support portion and the carbon substrate 4 can be minimized, and even when the entire surface of the carbon substrate 4 is coated with a tantalum carbide coating film, only one coating step is required. , The manufacturing cost can be reduced.

  However, in the vicinity of such a supporting point, although the tantalum carbide coating film is coated, the tantalum atom concentration becomes low. If such a location is inside the crucible 12 or the guide member 9, there is a concern that the quality of the SiC single crystal to be grown may be affected. Therefore, it is preferable to provide such a support location with a low concentration of tantalum atoms outside the crucible 12 or the guide member 9. In this way, the quality of the SiC single crystal to be grown is not affected.

Moreover, since the member for a semiconductor single crystal manufacturing apparatus is used repeatedly several times, it is preferable that the crystallinity of a tantalum carbide coating film does not mutate in the growth process of a semiconductor single crystal. For example, when growing a SiC single crystal by a sublimation recrystallization method, the tantalum carbide-coated film has a (200) plane even when heated to 2500 ° C. in an inert atmosphere of 1.0 × 10 ³ Pa or less. The intensity of the corresponding X-ray diffraction line is greater than the intensity of the X-ray diffraction lines corresponding to the other crystal planes, and the intensity ratio is 60% of the sum of the intensities of the X-ray diffraction lines corresponding to all crystal planes It is preferable that it is more than.

  Hereinafter, the present invention will be more specifically described by way of examples, but the present invention is not limited thereto.

Example 1
First, isotropic graphite is processed into a conical cylindrical shape (guide member 9), a bottomed cylindrical shape (crucible 12), a disk shape (susceptor 21), and a cylindrical shape (inner wall member 18), and these are carbon-based It was set as material 4. Arithmetic mean roughness Ra of the surface of these carbon base materials 4 was 0.5 micrometer.

  Next, the carbon substrate 4 was placed in the reaction chamber 2 of the external heating type low pressure CVD apparatus 1. The carbon substrate 4 was supported by a support means 5 having three supports with a pointed tip. At this time, the tip of the support portion is the outer surface of the truncated conical cylindrical carbon substrate 4, the outer surface of the carbon substrate 4 of the bottomed cylindrical shape, the lower surface of the disk shape, and the outer surface of the cylindrical shape. It was in contact with the surface.

Subsequently, tantalum pentachloride gasified by heating methane (CH ₄ ) gas to 0.5 SLM, raw material supply unit 6 as carrier gas, argon (Ar) gas to 1.5 SLM at a temperature of 120 to 220 ° C. TaCl ₅ ) was supplied at 0.1 SLM and reacted at a pressure of 10 to 100 Pa and at a temperature of 1100 ° C. in the reaction chamber 2 to form a tantalum carbide coating film with a film thickness of 30 μm on the entire surface of the carbon substrate 4.

  The carbon substrate 4 coated with the tantalum carbide coating film was taken out from the reaction chamber 2, and the crucible 12 made of the tantalum carbide coated carbon material, the guide member 9, the susceptor 21, and the inner wall member 18 were completed.

  About the produced crucible 12 and the guide member 9, 2 (theta) / (theta) measurement (out-of-plane) was performed using the XRD apparatus (RINT-2500VHF made from RIGAKU). As a result, the intensity of the X-ray diffraction line corresponding to the (200) plane of the tantalum carbide coating film is larger than the intensity of the X-ray diffraction line corresponding to other crystal planes, and the intensity ratio corresponds to all crystal planes It was found to be 96.4% with respect to the sum of the intensities of the X-ray diffraction lines.

  Moreover, arithmetic mean roughness Ra was measured about the tantalum carbide coating film surface using Mitsutoyo Co., Ltd. make surf test SJ-210. As a result, the arithmetic mean roughness Ra of the tantalum carbide coating film surface was 0.4 μm.

  Furthermore, the impurity concentration in the tantalum carbide coating film was evaluated by glow discharge mass spectrometry (GDMS). As a result, it was found that the tantalum carbide coating film contained 0.050 atm% of chlorine and 0.02 atm% of iron. This analysis is described in V.I. G. It carried out using Scientific VG9000, Element GD, Astrum. In addition, it was confirmed that the tantalum atom concentration was low around the three places in contact with the tip of the support portion.

  The crucible 12 and the guide member 9 which were produced in the decompression heating furnace 8 as shown in FIG. 2 were installed, and the SiC single crystal was grown by the sublimation recrystallization method. The SiC raw material 15 was placed in the crucible 12, and the SiC seed crystal 16 with a diameter of 2 inches was placed on the top of the raw material. Argon gas is introduced into the reduced pressure heating furnace 8 at 10 to 30 slm, the pressure is 500 to 1000 Pa, the temperature is 2000 to 2500 ° C., the SiC raw material 15 is sublimated, and a 5 mm thick SiC single crystal is formed on the SiC seed crystal 16 I grew up.

  The production of the SiC single crystal was repeated a plurality of times, and the number of times the SiC crystal adhered to the crucible 12 and the guide member 9 was confirmed. As a result, adhesion of the SiC crystal was confirmed after 23 times use, and the necessity of replacing with a new member arose.

The manufactured susceptor 21 and the inner wall member 18 were placed in a CVD apparatus 17 as shown in FIG. 3, and an SiC single crystal was epitaxially grown by the CVD method. An SiC single crystal substrate 24 processed into a substrate shape from a bulk single crystal was placed on the susceptor 21. Into the CVD apparatus, 30 sccm of monosilane (SiH ₄ ) and 70 sccm of propane (C ₃ H ₈ ) were introduced, and the pressure was 45 Torr and the temperature was 1550 ° C., and an SiC single crystal was epitaxially grown on the substrate.

  The production of the SiC single crystal was repeated a plurality of times, and the number of times that the SiC crystal adhered to the susceptor 21 and the inner wall member 18 was confirmed. As a result, adhesion of the SiC crystal was confirmed after 94 times of use, and it became necessary to replace with a new member. These conditions and results are shown in Table 1.

Example 2
The crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 are manufactured by the same method as in Example 1 except that the arithmetic mean roughness Ra of the surface of the carbon base 4 is 1.0 μm, and the evaluation is performed. The The results are shown in Table 1.

Example 3
The crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were produced and evaluated in the same manner as in Example 1 except that the arithmetic mean roughness Ra of the surface of the carbon substrate was 2.0 μm. . The results are shown in Table 1.

Example 4
A crucible 12, a guide member 9, a susceptor 21, and an inner wall member 18 are produced by the same method as in Example 1 except that the arithmetic mean roughness Ra of the surface of the carbon base 4 is 3.0 μm, and the evaluation is performed. The The results are shown in Table 1.

Example 5
The crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 are manufactured by the same method as in Example 1 except that the arithmetic mean roughness Ra of the surface of the carbon base 4 is 4.0 μm, and the evaluation is performed. The The results are shown in Table 1.

Example 6
First, the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were manufactured by the same method as in the third embodiment. The surface of the tantalum carbide coating film of the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 was roughened to have an arithmetic average roughness Ra of 3.8 μm. The evaluation was performed in the same manner as in Example 1. The results are shown in Table 1.

Example 7
First, the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were manufactured by the same method as in the third embodiment. The surface of the tantalum carbide coating film of the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 was roughened to have an arithmetic average roughness Ra of 3.4 μm. The evaluation was performed in the same manner as in Example 1. The results are shown in Table 1.

Example 8
First, the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were manufactured by the same method as in the third embodiment. The surface of the tantalum carbide coating film of the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 was roughened to have an arithmetic average roughness Ra of 2.8 μm. The evaluation was performed in the same manner as in Example 1. The results are shown in Table 1.

Example 9
First, the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were manufactured by the same method as in the third embodiment. The surface of the tantalum carbide coating film of the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 was roughened to have an arithmetic average roughness Ra of 2.2 μm. The evaluation was performed in the same manner as in Example 1. The results are shown in Table 1.

Example 10
First, the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were manufactured by the same method as in the third embodiment. Thereafter, annealing was performed at 2500 ° C. The evaluation was performed in the same manner as in Example 1. The results are shown in Table 1.

  It was found that the concentration of chlorine atoms in the tantalum carbide coating film of Example 10 was 0.009 atm%, the concentration of iron atoms was 0.10 atm%, and the iron content was higher compared to Example 3. The

Example 11
The crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were produced in the same manner as in Example 3 except that the film formation temperature of the tantalum carbide coating film was changed to 950 ° C. Thereafter, annealing was performed at 2500 ° C. The evaluation was performed in the same manner as in Example 1. The results are shown in Table 1.

  The tantalum carbide coated film of Example 11 had the intensity of the X-ray diffraction line corresponding to the (220) plane before the annealing treatment greater than the intensity of the X-ray diffraction line corresponding to the other crystal planes, but After treatment, the intensity of the X-ray diffraction line corresponding to the (200) plane becomes greater than the intensity of the X-ray diffraction line corresponding to the other crystal planes, and the intensity ratio is the X-ray diffraction line corresponding to the entire crystal plane It was 65.4% with respect to the sum of the intensity of. In addition, it was found that the annealing treatment showed that the concentration of chlorine atoms in the tantalum carbide coating was 0.009 atm%, the concentration of iron was 0.10 atm%, and the content of iron was larger than that in Example 3. The

Example 12
The crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were produced by the same method as in Example 3 except that the number of times of forming the tantalum carbide coating film was two, and the evaluation was performed. The results are shown in Table 1.

  At this time, film formation was performed while changing the support location of the carbon base material 4 between the first and second times. The tantalum atom concentration was not low around the three locations that were in contact with the tip of the support during the first deposition. In addition, although the concentration of tantalum atoms near the surface was low around the three locations that were in contact with the tip of the support during the second deposition, the concentration of tantalum atoms in the tantalum carbide coating film near the carbon substrate 4 was low. Was not getting lower.

Example 13
It was set as the structure which can rotate a base material by setting the rotational symmetry axis of a base material as a rotation axis, and the materials supply part was arranged on the extension of a rotation axis. Then, the film was formed while the substrate was rotated at a CH ₄ flow rate of 0.2 SLM and a film formation temperature of 1200 ° C. Except for this point, the crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured in the same manner as in Example 1 and evaluated. The results are shown in Table 1.

Example 14
Two sets of substrates were prepared in which the rotational symmetry axis of the substrate was made to rotate as a rotation axis. The rotation axes of the respective base materials were arranged on a revolving track with a rotation radius of 180 mm so that the rotation axes were at symmetrical positions with respect to the rotation axis, and the raw material supply portion was arranged on the extension of the rotation axis. Then, the film was formed while revolving each substrate while rotating at a CH ₄ flow rate of 0.75 SLM. Except for this point, the crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured in the same manner as in Example 1 and evaluated. The results are shown in Table 1.

Example 15
Two sets of substrates were prepared in which the rotational symmetry axis of the substrate was made to rotate as a rotation axis. The rotation axes of the respective base materials were arranged on a revolving track with a rotation radius of 180 mm so that the rotation axes were at symmetrical positions with respect to the rotation axis, and the raw material supply portion was arranged on the extension of the rotation axis. Then, the film was formed while making each substrate rotate while rotating at a CH ₄ flow rate of 1.0 SLM. Except for this point, the crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured in the same manner as in Example 1 and evaluated. The results are shown in Table 1.

Example 16
Two sets of substrates were prepared in which the rotational symmetry axis of the substrate was made to rotate as a rotation axis. The rotation axes of the respective substrates were disposed on a revolving track with a rotation radius of 180 mm so that the rotation axes of the respective substrates were at symmetrical positions with respect to the rotation axis. Then, the film was formed while revolving while rotating each substrate at a CH ₄ flow rate of 1.25 SLM. Except for this point, the crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured in the same manner as in Example 1 and evaluated. The results are shown in Table 1.

Example 17
Three sets of substrates were prepared in which the rotation symmetry axis of the substrate was made to rotate as a rotation axis. The rotation axes of the respective base materials were disposed at equal intervals (that is, at 120 ° intervals with respect to the revolution axis) on the orbit of 180 mm of revolution radius, and the raw material supply portion was disposed on the extension of the revolution axis. Then, the film was formed while revolving each substrate while rotating the flow rate of the CH ₄ at 2.0 SLM and the film forming temperature at 850 ° C. Except for this point, the crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured in the same manner as in Example 1 and evaluated. The results are shown in Table 1.

Example 18
Two sets of substrates were prepared in which the rotational symmetry axis of the substrate was made to rotate as a rotation axis. The rotation axes of the respective base materials are arranged on a revolving track with a rotation radius of 180 mm so that the rotation axes are symmetrical with respect to the rotation axis, and the material supply unit has an angle of 20 ° to the rotation axis It arranges so that the spout of a none and a raw material supply part may open on the extension of a revolution axis. Then, the film was formed while revolving while rotating each substrate with a CH ₄ flow rate of 0.1 SLM. Except for this point, the crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured in the same manner as in Example 1 and evaluated. The results are shown in Table 1.

Embodiment 19
Three sets of substrates were prepared in which the rotation symmetry axis of the substrate was made to rotate as a rotation axis. The rotation axis of each base material is equally spaced on the orbit of 180 mm of revolution radius (that is, at an interval of 120 ° with respect to the revolution axis), and the material supply unit makes an angle of 20 ° with the revolution axis and It arrange | positioned so that the jet nozzle of the raw material supply part might open 180 mm from the extension of the revolution axis. The film was formed while revolving each substrate while rotating at a CH ₄ flow rate of 4.0 SLM. Except for this point, the crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured in the same manner as in Example 1 and evaluated. The results are shown in Table 1.

Comparative Example 1
The crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 are manufactured by the same method as in Example 1 except that the arithmetic mean roughness Ra of the surface of the carbon base 4 is 4.5 μm, and the evaluation is performed. The The results are shown in Table 1.

Comparative Example 2
First, the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were manufactured in the same manner as in Comparative Example 1. The surface of the tantalum carbide coating film of the crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 was polished to have an arithmetic average roughness Ra of 1.8 μm. The evaluation was carried out in the same manner as in Example 1, and the results are shown in Table 1.

Comparative Example 3
The crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured in the same manner as in Example 3 except that the flow rate of CH ₄ gas was changed to 5 SLM, and the evaluation was performed. The results are shown in Table 1.

Comparative Example 4
The crucible 12, the guide member 9, the susceptor 21, and the inner wall member 18 were produced by the same method as in Example 3 except that the film formation temperature of the tantalum carbide coating film was changed to 950 ° C., and the evaluation was performed. The results are shown in Table 1.

Comparative Example 5
The crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured by the same method as in Example 3 except that the film formation temperature of the tantalum carbide coating film was changed to 750 ° C., and the evaluation was performed. The results are shown in Table 1.

Comparative Example 6
The crucible 12, the guide member 9, the susceptor 21 and the inner wall member 18 were manufactured and evaluated in the same manner as in Example 3 except that the flow rate of CH ₄ during film formation was changed to 0.09 SLM. The results are shown in Table 1.

  When the results of Examples 1 to 12 are compared with the results of Comparative Examples 1 to 4, the intensity of the X-ray diffraction line corresponding to the (200) plane of the tantalum carbide coating film is another The product life of the tantalum carbide-coated carbon material if the intensity is greater than or equal to 60% of the sum of the intensities of the X-ray diffraction lines corresponding to all crystal planes, which is greater than the intensity of the X-ray diffraction lines corresponding to crystal planes But it turned out to be long.

  From the results of Examples 1 to 5, by setting the arithmetic average roughness Ra of the surface of the carbon base 4 to 4.0 μm or less, the X-ray diffraction line corresponding to the (200) plane of the tantalum carbide coating film It has been found that the strength of is 60% or more of the sum of the strengths of X-ray diffraction lines corresponding to all crystal planes, and the product life of the tantalum carbide-coated carbon material can be extended.

  On the other hand, it is understood from the results of Examples 1 to 5 that the peel strength between the carbon substrate 4 and the tantalum carbide coating film also increases as the arithmetic mean roughness Ra of the surface of the carbon substrate 4 increases. The When the peel strength between the carbon base 4 and the tantalum carbide coating film is smaller than 1 MPa, the coating film is easily peeled off, which is not preferable for applying the tantalum carbide coated carbon material as a member for a semiconductor single crystal production device. In order to make the peel strength between the carbon substrate 4 and the tantalum carbide coating film 1 MPa or more, the arithmetic average roughness Ra of the surface of the carbon substrate 4 is preferably 0.4 μm or more, and 0.8 μm or more It is more preferable to

  From the results of Example 6 to Example 9, in order to prolong the product life of the tantalum carbide-coated carbon material used in the semiconductor single crystal production apparatus, it is preferable that Ra of the tantalum carbide coating film is smaller, and Ra should be 3. It can be said that it is more preferable to set it as 5 micrometers or less.

  Comparison of Comparative Example 1 and Comparative Example 2 shows that even if the intensity of the X-ray diffraction line corresponding to the (200) plane of the tantalum carbide coating film is the same, the tantalum coating film is polished, etc. It has been found that the product life is extended by reducing the arithmetic mean roughness Ra of the tantalum coating film.

  Comparing Example 3 and Comparative Example 4, in the step of coating tantalum carbide on the carbon substrate 4, tantalum carbide crystal coated thereon by making the temperature in the reaction chamber 2 larger than 1000 ° C. It has been found that the intensity of the X-ray diffraction line corresponding to the (200) plane of is increased, and the product life is accordingly extended. Further, comparing Example 17 and Comparative Example 5, when the flow ratio of methane to tantalum pentachloride is increased 20 times, the peak intensity of the (200) plane is obtained if the temperature in the reaction chamber 2 is 850 ° C. or higher. It turned out that it can be enlarged. On the other hand, if the reaction temperature is too high, the crystal system of tantalum carbide changes to needle crystals, and the peak intensity of the (200) plane decreases, so the reaction temperature is preferably 1200 ° C. or less. From the above results, in order to improve the product life of the tantalum carbide-coated carbon material, it was found that the temperature is preferably 850 ° C. or more and 1200 ° C. or less.

Comparing Example 11 with Comparative Example 4, in the step of annealing the tantalum carbide-coated carbon substrate 4, the temperature of the annealing is set to 2500 ° C. to cope with the (200) plane of tantalum carbide crystal. It was found that the intensity of the X-ray diffraction line increases and the product life becomes longer.
From the above results, it has been found that the annealing temperature is preferably 2500 ° C. in order to improve the product life of the tantalum carbide-coated carbon material.

Comparing Example 3 and Comparative Example 3, when the proportion of tantalum pentachloride in the source gas is low, the peak intensity of the (200) plane tends to decrease, and the flow ratio of methane to tantalum pentachloride in the source gas It was found that (CH ₄ / TaCl ₅ ) should be about 5. Further, from the results of Examples 13 to 19 and Comparative Example 6, the flow rate ratio of methane and tantalum pentachloride in the raw material gas _(CH 4 / TaCl ₅₎ it was found that or equal to 2 or more and 20 or less.

  The present invention is not limited to the above embodiment. The above-described embodiment is an exemplification, and the present invention has the substantially same constitution as the technical idea described in the claims of the present invention, and the same effects can be exhibited by any invention. It is included in the technical scope of

DESCRIPTION OF SYMBOLS 1 External heating type low pressure CVD apparatus 2 Reaction chamber 3 Heater 4 Carbon substrate 5 Support means 6 Raw material supply part 7 Exhaust part 8 Reduced pressure heating furnace 9 Guide member 10 Guide member inner surface 11 Guide member outer surface 12 crucible 13 crucible inner surface 14 Crucible outer surface 15 SiC raw material 16 SiC seed crystal 17 external heat type low pressure CVD apparatus 18 inner wall member 19 inner wall member inner surface 20 inner wall member outer surface 21 susceptor 22 susceptor inner surface 23 susceptor outer surface 24 SiC single crystal substrate

Claims (17)

A tantalum carbide-coated carbon material, wherein at least a part of the surface of a carbon substrate is coated with a tantalum carbide-based coating film containing tantalum carbide as a main component,
In the tantalum carbide coating film, the intensity of the X-ray diffraction line corresponding to the (200) plane in the out-of-plane direction is larger than the intensity of the X-ray diffraction line corresponding to the other crystal planes. A tantalum carbide-coated carbon material, which is 60% or more of the sum of the intensities of X-ray diffraction lines corresponding to.   Arithmetic mean roughness Ra of the said tantalum carbide coating film surface is 3.5 micrometers or less, The tantalum carbide coated carbon material of Claim 1 characterized by the above-mentioned.   Arithmetic mean roughness Ra of the said carbon base-material surface is 4.0 micrometers or less, The tantalum carbide coated carbon material of Claim 1 or 2 characterized by the above-mentioned.   The carbonization according to any one of claims 1 to 3, wherein the number of tantalum atoms contained in the tantalum carbide coating film is greater than the number of carbon atoms and 1.2 times or less the number of carbon atoms. Tantalum-coated carbon material.   The tantalum carbide-coated carbon material according to claim 1, wherein the tantalum carbide coating film contains chlorine atoms at an atomic concentration of 0.01 atm% or more and 1.00 atm% or less. A member for a semiconductor single crystal production apparatus, comprising a tantalum carbide-coated carbon material coated with a tantalum carbide-based coating film containing tantalum carbide as a main component of at least a part of a carbon substrate surface,
In the tantalum carbide coating film, the intensity of the X-ray diffraction line corresponding to the (200) plane in the out-of-plane direction is larger than the intensity of the X-ray diffraction line corresponding to the other crystal plane A member for a semiconductor single crystal production apparatus, characterized in that it is 60% or more with respect to the sum of the intensities of X-ray diffraction lines corresponding to the surface.   The member for a semiconductor single crystal production device according to claim 6, wherein the member for a semiconductor single crystal production device is used for a production device of SiC single crystal.   The said semiconductor single crystal manufacturing apparatus member is a crucible or a guide member used for an apparatus for manufacturing a SiC single crystal by a sublimation recrystallization method, for a semiconductor single crystal manufacturing apparatus according to claim 7, Element.   The semiconductor single crystal according to claim 7, wherein the member for a semiconductor single crystal manufacturing device is a susceptor or an inner wall member used for a device for epitaxially growing a SiC single crystal by a chemical vapor deposition method. A member for a crystal manufacturing apparatus.   The semiconductor single crystal manufacturing apparatus according to any one of claims 6 to 9, wherein the member for manufacturing a semiconductor single crystal has two or more locations having a low concentration of tantalum atoms on the surface of the tantalum carbide coating film. A member for a crystal manufacturing apparatus. Preparing a carbon substrate having an arithmetic surface roughness Ra of 4.0 μm or less;
Coating at least a part of the surface of the carbon substrate with a tantalum carbide coating film.   The method for producing a tantalum carbide-coated carbon material according to claim 11, wherein the tantalum carbide coating film is coated while the carbon base material is rotated about a rotation axis.   The method for producing a tantalum carbide-coated carbon material according to claim 12, wherein the tantalum carbide film is coated while revolving the revolving shaft around a revolving shaft. The step of preparing is
Supporting the carbon substrate in a reaction chamber,
The coating step is
Supplying a source gas containing a compound containing a carbon atom and tantalum halide into the reaction chamber;
14. A process for producing a tantalum carbide-coated carbon material according to any one of claims 11 to 13, comprising the step of reacting the supplied source gas by a thermal CVD method to form the tantalum carbide coating film. Method.   The method for producing a tantalum carbide-coated carbon material according to claim 14, wherein the temperature in the reaction chamber is set to 850 ° C. or more and 1200 ° C. or less in the step of supplying the raw material gas. In the step of supplying the source gas, the compound containing carbon atoms is methane (CH ₄ ), and the halogenated tantalum is tantalum pentachloride (TaCl ₅ ), and the flow ratio of methane to tantalum pentachloride supplied is 2 The method for producing a tantalum carbide-coated carbon material according to claim 14 or 15, characterized in that it is not less than 20 and not more than 20.   The tantalum carbide-coated carbon material according to any one of claims 11 to 16, further comprising a step of annealing the carbon substrate on which the tantalum carbide coating film is formed after the coating step. Manufacturing method.

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