PBN container and method for manufacturing the same

Abstract

The present invention provides a PBN container having excellent durability, which is a container in which a conductive film is laminated on the surface of a container body formed by laminating PBN, and a method for manufacturing such a PBN container. [Solution] A PBN container comprising a container body made of a laminate of pyrolytic boron nitride and a conductive film covering the surface of the container body, characterized in that the angle θ formed by the layer cross-section of the container body and the inner wall surface or outer wall surface of the container body that is in contact with the layer cross-section is 20° or more and 80° or less around the entire circumference of the opening of the container body, and the tip portion of the opening of the container body has a shape in which the radius of curvature R is 0.2 mm or more and 3.0 mm or less around the entire circumference of the opening of the container body.

Description

[Technical Field]

[0001] The present invention relates to a PBN container and a method for manufacturing a PBN container. [Background technology]

[0002] PBN (pyrolytic boron nitride, or pyrolytic boron nitride) is produced using a pyrolysis method. Therefore, when viewed microscopically, it has a type of laminated film structure. The laminated film has anisotropy in both the plane and thickness directions. This type of PBN has various advantages, such as the ease with which high-purity containers can be formed using methods such as CVD, and the prevention of container-related contamination. For this reason, PBN is used as a material for a variety of containers, including hearth liners for electron beam evaporation, MBE (molecular beam epitaxy) containers, metal melting containers, and analytical containers.

[0003] Here, a hearth liner for electron beam evaporation will be used as an example of a PBN container for explanation. Electron beam evaporation is a useful method for forming a thin film on a substrate. In electron beam evaporation, an electron beam is irradiated onto an evaporation material to heat and evaporate the material, and the evaporated material is then deposited onto a substrate to form a thin film on the substrate (see, for example, Non-Patent Document 1). For example, a hearth liner for electron beam evaporation is placed in a water-cooled copper crucible (hearth), and an electron beam is irradiated from an electron gun onto the evaporation material filled in the hearth liner to evaporate the evaporation material.

[0004] In this case, it is possible to fill the hearth directly with the evaporation material without using a hearth liner for electron beam evaporation. However, the hearth liner can be removed for cleaning, which makes cleaning easy. Furthermore, when a different evaporation material is to be evaporated onto the substrate, it is only necessary to replace the hearth liner, which is simple and prevents contamination. For these reasons, a hearth liner for electron beam evaporation is usually used.

[0005] 5 is a schematic cross-sectional view showing an example of a hearth liner and hearth for electron beam evaporation. This hearth liner for electron beam evaporation (PBN container) 50 is housed in a copper hearth 51, and its bottom is in contact with the hearth 51. The hearth 51 is cooled with cooling water 52. As shown in FIG. 5, the hearth liner 50 is filled with a deposition material 53 such as aluminum.

[0006] Known hearth liners for electron beam evaporation include those made of PBN and carbon. However, carbon hearth liners have the problem of reacting with the evaporation material. For example, if aluminum is filled into a carbon hearth liner and electron beam evaporation is performed, the carbon and aluminum react to produce aluminum carbide (Al4C3). This results in a decrease in the crystallinity and purity of the aluminum thin film evaporated onto the substrate.

[0007] In contrast, hearth liners made of PBN have the advantage of being less reactive with the deposition material. However, even when using a PBN hearth liner, the following problems still exist. First, the deposition material can only be partially melted in the immediate vicinity of the electron beam irradiation, not completely melted. Furthermore, when aluminum is used as the deposition material, surface tension causes the aluminum to creep up along the inner wall of the hearth liner, making it difficult to observe the melted state and leaving poor quality melt marks. Furthermore, because PBN is insulating, it causes charge buildup when irradiated with an electron beam. For these reasons, it has been impossible to stably deposit large-area, uniform, high-purity metal films.

[0008] To solve this problem, a PBN hearth liner has been devised, in which a conductive film is laminated on the surface of a container body formed by laminating PBN (see, for example, Patent Document 1). When this PBN hearth liner is used, the conductive film is heated by an electron beam, allowing the deposition material to melt entirely. In addition, the presence of the conductive film eliminates the problem of charge-up. Furthermore, it is difficult for the molten deposition material, such as aluminum, to creep up the inner wall surface of the hearth liner. For this reason, it is believed that the use of this PBN hearth liner makes it possible to stably produce uniform, high-purity metal films over a large area.

[0009] However, hearth liners, which consist of a PBN laminated container body with a conductive film laminated on its surface, are prone to breakage and have a short lifespan, which has led to a demand for PBN containers with excellent durability. [Prior art documents] [Patent documents]

[0010] [Patent Document 1] Japanese Patent Application Publication No. 9-59766 [Patent Document 2] Japanese Patent Application Laid-Open No. 2006-104554 [Non-patent literature]

[0011] [Non-Patent Document 1] "Thin Film Engineering Handbook" Ohmsha, p. 101-p. 105, published December 10, 1983 Summary of the Invention [Problem to be solved by the invention]

[0012] The present invention has been made in consideration of such problems, and aims to provide a PBN container having excellent durability, in which a conductive film is laminated on the surface of a container body formed by laminating PBN, and a method for manufacturing such a PBN container. [Means for solving the problem]

[0013] In order to solve the above problems, the present invention provides a PBN container comprising a container body made of a pyrolytic boron nitride (PBN) laminate and a conductive film covering the surface of the container body, wherein the angle θ formed by the layer cross-section of the container body and the inner wall surface or outer wall surface of the container body that is in contact with the layer cross-section is 20° or more and 80° or less over the entire circumference of the opening of the container body, and the tip portion of the opening of the container body has a shape in which the radius of curvature R is 0.2 mm or more and 3.0 mm or less over the entire circumference of the opening of the container body.

[0014] Due to its shape, such a PBN container makes it more difficult for the conductive film to peel off, and can be made highly durable.

[0015] In this case, the PBN container of the present invention preferably has a flat surface at the tip of the opening of the container body, and the length of the flat surface in the radial direction of the container body is 0.05 mm or more and 2 mm or less.

[0016] By having such a flat surface, the conductive film is more resistant to peeling, and durability is improved.

[0017] In addition, the density of the container body is 1.7 g / cm 3 More than 2.2g / cm 3 It is preferable that:

[0018] By making the container body have such a density, it becomes difficult for the molten metal material (for example, vapor deposition material such as aluminum) to penetrate into the PBN layer, improving durability.

[0019] Furthermore, it is preferable that the surface roughness Ra of the container body is in the range of 0.5 μm or more and 5.0 μm or less.

[0020] By providing such surface roughness, it is possible to optimize the surface tension, which makes it difficult for metal materials (for example, evaporation materials such as aluminum) to creep up the inner wall surface of the PBN container.

[0021] It is also preferable that the surface roughness Ra of the outer wall side of the container body is smaller than the surface roughness Ra of the inner wall side of the container body.

[0022] By doing so, even if the metal material (for example, evaporation material such as aluminum) creeps up the inner wall surface of the PBN container, it can be prevented from leaking out to the outer wall surface.

[0023] It is also preferable that the angle θ′ formed between the inner wall surface or outer wall surface of the container body and the axis of symmetry of the container body is 0.5° or more and 60° or less.

[0024] By using such a shape, the amount of metal material (for example, vapor deposition material such as aluminum) that creeps up the inner wall surface of the PBN container can be optimized, improving product quality.

[0025] The PBN container is preferably a PBN hearth liner for electron beam evaporation.

[0026] As described above, the PBN container of the present invention has excellent durability. Therefore, when used as a PBN hearth liner for electron beam evaporation, it is possible to deposit a uniform, high-purity metal film over a large area over a long period of time. Furthermore, because it is resistant to breakage and has a long life, it requires fewer replacements, does not reduce the operating rate of the equipment, and has the effect of reducing costs.

[0027] The conductive film is preferably made of pyrolytic graphite (PG).

[0028] Like PBN, pyrolytic graphite (PG) can be easily formed into a high-purity film using methods such as CVD, and it does not easily react with filler materials such as molten metal. PG also has excellent electrical conductivity. These factors make it suitable for use as a conductive film.

[0029] The conductive film preferably has a thickness of 5 μm or more and 100 μm or less.

[0030] By using a conductive film with such a thickness, the durability and yield of the container can be improved.

[0031] The present invention also provides a method for manufacturing a PBN container, which includes the steps of forming a container body by stacking pyrolytic boron nitride and processing the shape, and stacking a conductive film on the surface of the container body, wherein in the step of forming the container body, the angle θ between the layer cross-section of the container body and the inner wall surface or outer wall surface of the container body that is in contact with the layer cross-section is 20° or more and 80° or less around the entire circumference of the opening of the container body, and the tip portion of the opening of the container body has a shape in which the radius of curvature R is 0.2 mm or more and 3.0 mm or less around the entire circumference of the opening of the container body.

[0032] Such a method for manufacturing a PBN container makes it possible to manufacture a PBN container in which the conductive film is less likely to peel off and which has high durability.

[0033] In this case, the PBN container to be manufactured is preferably a PBN hearth liner for electron beam evaporation.

[0034] Thus, the method for manufacturing a PBN container of the present invention can be suitably employed for manufacturing a PBN hearth liner for electron beam evaporation.

[0035] The conductive film is preferably made of pyrolytic graphite.

[0036] Like PBN, PG can be easily formed into a high-purity film using methods such as CVD, and it does not easily react with filler materials such as molten metal. PG also has excellent electrical conductivity. These factors make it suitable for use as a conductive film. [Effects of the Invention]

[0037] As described above, the PBN container and its manufacturing method of the present invention provide a PBN container having a conductive film laminated on the surface of a container body formed by laminating PBN. The angle between the cross section of the container body and at least one wall surface tangent to the cross section of the layer is 20° to 80°, and the tip of the opening of the container body has a shape with a radius of curvature R of 0.2 mm to 3.0 mm. This makes it difficult for residual stress to occur during use of the PBN container, making it less likely to break. Therefore, the present invention makes it possible to provide a PBN container with excellent durability. [Brief explanation of the drawings]

[0038] [Figure 1] 1A and 1B are schematic diagrams showing an example of a PBN container (hearth liner for electron beam evaporation) of the present invention, in which (a) is a cross-sectional view and (b) is an enlarged view thereof. [Figure 2] FIG. 2 is a schematic cross-sectional view showing another example of the PBN container (hearth liner for electron beam evaporation) of the present invention. [Figure 3] FIG. 10 is a schematic cross-sectional view showing still another example of the PBN container (hearth liner for electron beam evaporation) of the present invention. [Figure 4] 1 is an explanatory diagram showing a method for manufacturing a PBN container according to the present invention. [Figure 5] FIG. 1 is a schematic cross-sectional view showing an example of a general hearth liner and hearth for electron beam evaporation. DETAILED DESCRIPTION OF THE INVENTION

[0039] The present invention will be described below.

[0040] PBN and conductive films have significantly different thermal expansion coefficients. Therefore, if the angle between the layer cross-section and the wall surface of a PBN container body is approximately 90°, as in a typical PBN container, residual stress acts between the PBN and the conductive film at the layer cross-section upon heating and cooling, exerting a force that separates the PBN layers. As a result, repeated heating and cooling of the container causes peeling to progress, and the molten deposition material creeps up and seeps into the layer, damaging the container. Therefore, as in Patent Document 2, a PBN container is designed such that the angle between the layer cross-section of the body and at least one wall surface in contact with the layer cross-section is set to 20° to 80°, thereby reducing the apparent thermal expansion coefficient of the PBN at the layer cross-section. This makes it less likely for residual stress to occur even when the container is repeatedly heated and cooled, and prevents damage to the container over a long period of time. In the PBN container of the present invention, in addition to the above-mentioned shape, it has been discovered that by making the shape of the tip of the container opening fall within the range of R0.2 mm or more and R3.0 mm or less around the entire circumference of the container opening, the conductive film is less likely to peel off and durability is improved.

[0041] In other words, the PBN (pyrolytic boron nitride) container of the present invention is a PBN container comprising a container body made of a laminate of pyrolytic boron nitride and a conductive film covering the surface of the container body, wherein the angle θ formed by the layer cross-section of the container body and the inner wall surface or outer wall surface of the container body that is in contact with the layer cross-section is 20° or more and 80° or less around the entire circumference of the opening of the container body, and the tip portion of the opening of the container body has a shape in which the radius of curvature R is 0.2 mm or more and 3.0 mm or less around the entire circumference of the opening of the container body.

[0042] The PBN container of the present invention was made possible by the following findings: The inventors conducted extensive research to improve the durability of a PBN container in which a conductive film is laminated on the surface of a container body formed by laminating PBN.

[0043] Here, the conductive film can be, for example, PG (pyrolytic graphite or pyrolytic graphite). The thermal expansion coefficients of PG used as the conductive film and PBN used as the container body are significantly different, and it is also known that the thermal expansion coefficient of PBN itself differs significantly between the surface direction and the thickness direction. The thermal expansion coefficients of PBN and PG are shown below. PG expansion rate 2×10 -6 [ / ℃] PBN surface expansion coefficient 3×10 -6 [ / ℃] PBN thickness expansion coefficient 25×10 -6 [ / ℃]

[0044] Such a large difference in thermal expansion coefficients causes the following problem. In conventional PBN containers, in which the angle between the layer cross-section (thickness cross-section) of the container body and the wall surface in contact with the layer cross-section is approximately 90°, the layer cross-section has a large expansion coefficient when cooled to room temperature after heating, which generates large residual stress in the layer cross-section. After several uses, the residual stress causes peeling and the molten vapor deposition material to creep up and seep in, resulting in damage at the opening. This shortens the lifespan of the PBN container.

[0045] Therefore, as a result of intensive research, the inventors have found that in order to suppress the occurrence of residual stress, the layer cross section of the main body is angle-cut so that the angle between the layer cross section and at least one wall surface that contacts the layer cross section is 20 to 80°, and the tip of the container opening is shaped to be within the range of R0.2 mm to R3.0 mm over the entire circumference of the container opening, and the apparent linear expansion coefficient of the layer cross section is 25 × 10 -6 The inventors have come up with the idea that it is sufficient to make the temperature smaller than [ / °C], and have completed the present invention.

[0046] Hereinafter, embodiments of the present invention will be described with reference to the drawings, but the present invention is not limited to these.

[0047] A cross-sectional view of an example of a PBN container of the present invention is shown in Figure 1. More specifically, Figure 1 shows an example of a hearth liner for electron beam evaporation as a PBN container. Figure 1(a) is a cross-sectional view, and Figure 1(b) is an enlarged view thereof.

[0048] The PBN container (hearth liner) 10 shown in FIG. 1 includes a container body 11 made of a PBN laminate and a conductive film 12 covering the surface of the container body 11. That is, the container is formed by laminating PBN and laminating the conductive film 12 on the surface of the container body 11. Furthermore, the angle θ between the layer cross section 13 of the container body 11 and the inner wall surface 14 or outer wall surface 15 of the container body 11 that contacts the layer cross section 13 is 20° or more and 80° or less around the entire circumference of the opening of the container body 11. In this case, the angle θ between the inner wall surface 16 of the container 10 covered with the conductive film 12 and the upper end surface 17 is also substantially the same as θ, 20° to 80°. This shape reduces the apparent thermal expansion coefficient of PBN, making it less likely for residual stress to occur in the layer cross section even when the container is repeatedly heated and cooled.

[0049] Furthermore, as shown in Figure 1, the tip of the opening of the container body 11 (portion 18 on the inner wall side of the container opening tip in Figure 1) has a shape with a radius of curvature R of 0.2 mm to 3.0 mm around the entire circumference of the opening of the container body. By making portion 18 on the inner wall side of the container opening tip rounded in this way, the apparent thermal expansion coefficient of PBN is reduced, and even when the container is repeatedly heated and cooled, residual stress is less likely to occur in the layer cross section, and the container will not break over a long period of time. The radius of curvature of the rounded shape here is 0.2 mm to 3 mm, preferably 0.3 mm to 1 mm, and even more preferably 0.4 mm to 0.75 mm.

[0050] The PBN container 10 of the present invention, which combines the above-described shapes, has improved durability and is less susceptible to peeling of the conductive film 12. Specifically, the apparent thermal expansion coefficient of PBN is reduced, and even when the container is repeatedly heated and cooled, residual stress is less likely to occur in the layer cross section, and the container will not break over a long period of time. This results in a container with excellent durability. Therefore, when electron beam evaporation is performed using this hearth liner for electron beam evaporation, stable film growth can be achieved over a long period of time. Furthermore, because it is less susceptible to breakage and has a long life, there is no reduction in the operating rate of the equipment due to replacement, which has the effect of reducing costs.

[0051] In the PBN container 10 of the present invention, as shown in Fig. 1, the angle θ formed between the layer cross section 13 of the container body 11 and the inner wall surface 14 in contact with the layer cross section 13 is preferably 20° to 80°. When a material is filled into the PBN container 10, the filler material, such as molten metal, may creep up the inner wall surface of the PBN container 10 due to surface tension and the like, and leak to the outside. However, if the angle formed between the layer cross section 13 and the inner wall surface 14 in contact with the layer cross section 13 is 20° to 80° as in the present invention shown in Fig. 1, the filler material is less likely to creep up the inner wall surface of the PBN container 10, and leakage of the filler material to the outside of the PBN container 10 can be more effectively prevented.

[0052] However, the angle θ between the outer wall surface 15 and the layer cross section 13 of the container body 11, of the inner wall surface 14 or outer wall surface 15 of the container body 11 that contacts the layer cross section 13, may be 20° or more and 80° or less over the entire circumference of the opening of the container body 11. In this case, although there is no effect of preventing leakage of the filling material, the effect of preventing breakage and the like and making the PBN container 10 highly durable can be obtained in the same manner as above.

[0053] In the PBN container 10 of the present invention, the angle θ formed between the layer cross section 13 of the container body 11 and the inner wall surface 14 or outer wall surface 15 of the container body 11 that contacts the layer cross section 13 (i.e., the angle substantially the same as the angle formed between the inner wall surface 16 and the upper end surface 17 of the PBN container 10) is set to 50° or less, thereby more reliably suppressing the generation of stress. On the other hand, by setting the angle θ to 40° or more, the mechanical strength of the PBN container 10 after angle cutting can be more sufficiently maintained. Therefore, it is more preferable that the angle θ be set to 40° or more and 50° or less.

[0054] 2, the angle may be changed to become steeper midway along the layer cross section 13. While θ1 and θ2 are shown in Fig. 2, the angle θ2 between the layer cross section 13 and the wall surface (inner wall surface 14 or outer wall surface 15) after the angle is changed is preferably set to 20° to 80°.

[0055] As shown in FIG. 3, the layer cross section 13 (upper end surface 17) may be an arc with a continuously changing angle (R-shaped: for example, a radius of curvature of about R10 mm to R1000 mm).

[0056] Furthermore, as shown in FIG. 1(b), the PBN container of the present invention preferably has a flat surface 19 at the tip of the opening of the container body 11, and the length of the flat surface 19 in the radial direction of the container body 11 is 0.05 mm or more and 2 mm or less. This shape makes the conductive film 12 even less likely to peel off, improving durability. It also reduces processing time during manufacturing, which is expected to improve productivity. As described above, the length of the flat surface 19 in the radial direction is preferably 0.05 mm or more and 2 mm or less, more preferably 0.1 mm or more and 1 mm or less, and particularly preferably 0.2 mm or more and 0.5 mm or less.

[0057] In addition, in the PBN container 10 of the present invention, the density of the container body 11 is 1.7 g / cm 3 More than 2.2g / cm 3By setting the density at such a level, it becomes difficult for the molten metal material (for example, a vapor deposition material such as aluminum) to penetrate into the PBN layer of the container body 11, improving durability. The density of the container body 11 is 1.7 g / cm as described above. 3 More than 2.2g / cm 3 The following range is preferred: 1.8 g / cm 3 More than 2.15g / cm 3 More preferably, 1.9 g / cm 3 More than 2.1g / cm 3 The following are particularly preferred:

[0058] Furthermore, the surface roughness Ra of the container body 11 is preferably in the range of 0.5 μm to 5.0 μm. When a material is filled into a conventional PBN container, the filling material, such as molten metal, may creep up the inner wall surface of the container due to surface tension and leak out. In the PBN container 10 of the present invention, by setting the surface roughness of the container body 11 within the above range, the surface tension is optimized, making it difficult for the deposition material, such as molten aluminum, to creep up the inner wall surface of the PBN container 10 (hearth liner). As described above, the surface roughness Ra of the container body 11 is preferably in the range of 0.5 μm to 5.0 μm, more preferably 1.0 μm to 3.0 μm, and particularly preferably 1.5 μm to 2.5 μm.

[0059] Furthermore, in the PBN container 10 of the present invention, the surface roughness Ra of the outer wall side of the container body 11 is preferably smaller than the surface roughness Ra of the inner wall side of the container body 11. This prevents the molten aluminum or other deposition material from leaking to the outer wall surface even if it creeps up the inner wall surface of the PBN container 10 (hearth liner). The difference between the surface roughness Ra of the outer wall side and the surface roughness Ra of the inner wall side of the container body 11 is preferably 0.1 μm or more and 4.5 μm or less, and more preferably 0.5 μm or more and 4.0 μm or less.

[0060] Furthermore, in the PBN container 10 of the present invention, the angle θ' between the inner wall surface 14 or outer wall surface 15 of the container body 11 and the axis of symmetry of the container body is preferably 0.5° or more and 60° or less. This optimizes the amount of deposition material, such as molten aluminum, that creeps up the inner wall surface of the PBN container 10 (hearth liner), improving product quality. This angle θ' is preferably 0.5° or more and 60° or less, more preferably 1.0° or more and 5.0° or less, and particularly preferably 2.0° or more and 4.0° or less.

[0061] Furthermore, the PBN container 10 of the present invention is preferably a PBN hearth liner for electron beam evaporation. As described above, the PBN container of the present invention has excellent durability. Therefore, when used as a PBN hearth liner for electron beam evaporation, it is possible to deposit a uniform, high-purity metal film over a large area over a long period of time. Furthermore, because it is resistant to breakage and has a long life, it requires fewer replacements, does not reduce the operating rate of the equipment, and has the effect of reducing costs.

[0062] Furthermore, in the PBN container 10 of the present invention, the conductive film 12 is preferably pyrolytic graphite (PG). Like PBN, pyrolytic graphite (PG) can be easily formed into a high-purity film by CVD or other methods, and it is also less likely to react with filler materials such as molten metal. PG also has excellent conductivity. PG is also less likely to contaminate filler materials and can reliably prevent charge-up. For these reasons, it is suitable as the conductive film 12 for the PBN container 10.

[0063] Furthermore, the thickness of the conductive film 12 is preferably 5 μm or more and 100 μm or less. If the thickness of the conductive film 12 is 5 μm or more, it is possible to prevent molten metal such as aluminum from penetrating into the PBN base material, thereby improving the durability of the PBN container 10. On the other hand, if the thickness is 100 μm or less, it is possible to prevent peeling due to the difference in thermal expansion coefficient between PG and PBN, thereby increasing the yield. Therefore, the thickness of the conductive film 12 is preferably 5 μm or more and 100 μm or less, more preferably 10 μm or more and 30 μm or less, and even more preferably 15 μm or more and 25 μm or less.

[0064] In the above, the PBN container of the present invention has been described as being used as a hearth liner for electron beam evaporation, but it may also be used as other containers such as a container for MBE (molecular beam epitaxy), a container for metal melting, or a container for analysis.

[0065] The present invention provides a method for manufacturing a PBN container that can produce the above-described PBN container 10. Specifically, the method includes the steps of forming a container body by stacking pyrolytic boron nitride and processing the shape, and stacking a conductive film on the surface of the container body, wherein in the step of forming the container body, the angle θ between the layer cross-section of the container body and the inner or outer wall surface of the container body that is in contact with the layer cross-section is 20° or more and 80° or less along the entire circumference of the opening of the container body, and the tip of the opening of the container body has a shape with a radius of curvature R of 0.2 mm or more and 3.0 mm or less along the entire circumference of the opening of the container body.

[0066] A method for manufacturing such a PBN container of the present invention can be performed, for example, as follows (FIG. 4). The step of forming a container body by stacking pyrolytic boron nitride and processing the shape can be performed as follows. First, a heat-resistant substrate 41 shaped to obtain a container of the desired shape is prepared. PBN is vapor-deposited onto the heat-resistant substrate 41 by a method such as CVD to form a PBN layer 40. After the vapor deposition reaction is complete, the substrate is cooled to room temperature and removed from the furnace (FIG. 4(a)). During this cooling process, a gap forms between the heat-resistant substrate 41 and the PBN layer 40 due to the difference in their respective thermal expansion coefficients. This gap can be used to pull out and separate the PBN layer 40 from the heat-resistant substrate 41. The pulled PBN layer 40 is then cut to an appropriate height to obtain the container body 42 (FIG. 4(b)). Furthermore, as shown in FIG. 4(c), the cross section of the layer of the manufactured container body 42 is processed to satisfy the angle θ and the radius of curvature R of the R portion of the container body of the present invention. Here, the layer cross section of the container body 42 may be machined so that the angle between the layer cross section and the inner wall surface is 20° to 80°, or conversely, the angle between the layer cross section of the container body 42 and the outer wall surface may be machined so that the angle between the layer cross section and the outer wall surface is 20° to 80°.

[0067] After processing the cross section of the layer, the main body 42 is placed in the CVD furnace again, and the surface of the main body 42 is coated with a conductive film 43 (FIG. 4(d)). When PG is used as the conductive film 43, a carbon source gas such as hydrocarbon or carbon chloride may be introduced into the CVD furnace.

[0068] In this manner, the PBN container 10 shown in FIG. 1 can be manufactured. [Example]

[0069] EXAMPLES The present invention will be specifically explained below with reference to examples and comparative examples, but the present invention is not limited to the following examples.

[0070] Example 1 A tapered cylindrical carbon mold 41 with a diameter of 50 mm and an angle θ' (the angle θ' between the plane defining the inner wall surface of the container body and the axis of symmetry of the mold) of 3.0° was placed in a CVD furnace, the temperature was kept at 1900°C, and ammonia as a nitrogen source and boron trichloride as a boron source gas were introduced at 3 L / min and 1 L / min, respectively, to deposit a 1 mm thick PBN layer 40 (Figure 4(a)). After cooling, the deposited PBN layer 40 was removed from the carbon mold 41 and cut to a height of 25 mm to produce the body 42 (Figure 4(b)).

[0071] The cross section of the fabricated main body 42 was then processed and polished so that the angle between the cross section and the inner wall surface in contact with the cross section was 80°, the R shape of the inner wall tip was 0.5 mm, the length of the flat surface at the tip was 0.2 mm, and the surface roughness was 2.0 μm on the inner wall surface and 1.5 μm on the outer wall surface (FIG. 4(c)). After processing and polishing, the main body 42 was placed again in the CVD furnace, kept at 2000°C, and propane gas as a carbon source was introduced at 3 L / min, and a 30 μm-thick PG layer 43 was laminated on the surface of the main body 42 (FIG. 4(d)). The density of the main body 42 was calculated by the immersion method and was found to be 1.9 g / cm 3 It was.

[0072] The PBN hearth liner 44 thus fabricated was actually used in electron beam evaporation. Specifically, 10 g of aluminum was loaded into the PBN hearth liner, and an electron beam was irradiated while sweeping to deposit an aluminum thin film on the substrate. When half of the aluminum loaded into the PBN hearth liner was used, it was reloaded with aluminum and used again to deposit an aluminum thin film. This process was repeated until the container had been used 105 times, at which point aluminum penetration was observed from the top surface of the container.

[0073] Example 2 A PBN hearth liner was fabricated in the same manner as in Example 1, except that the layer cross section of the main body was processed and polished so that the angle between the layer cross section and the inner wall surface in contact with the layer cross section was 50°. The evaluation results are shown in Table 1.

[0074] Example 3 A PBN hearth liner was fabricated in the same manner as in Example 1, except that the layer cross section of the main body was processed and polished so that the angle between the layer cross section and the inner wall surface in contact with the layer cross section was 20°. The evaluation results are shown in Table 1.

[0075] Example 4 A PBN hearth liner was produced in the same manner as in Example 2, except that the cross section of the body was processed and polished so that the R shape of the inner wall tip was 0.2 mm. The evaluation results are shown in Table 1.

[0076] Example 5 A PBN hearth liner was produced in the same manner as in Example 2, except that the cross section of the body was processed and polished so that the R shape of the inner wall tip was 3.0 mm. The evaluation results are shown in Table 1.

[0077] Example 6 A PBN hearth liner was produced in the same manner as in Example 2, except that the cross section of the body was processed and polished so that the length of the flat surface at the tip was 0.1 mm. The evaluation results are shown in Table 1.

[0078] Example 7 A PBN hearth liner was produced in the same manner as in Example 2, except that the cross section of the body was processed and polished so that the length of the flat surface at the tip was 3.0 mm. The evaluation results are shown in Table 1.

[0079] Example 8 By adjusting the reaction conditions, the density of the main body was 1.7 g / cm 3 Except for this, a PBN hearth liner was produced in the same manner as in Example 2. The evaluation results are shown in Table 1.

[0080] Example 9 By adjusting the reaction conditions, the density of the main body was 2.2 g / cm 3 Except for this, a PBN hearth liner was produced in the same manner as in Example 2. The evaluation results are shown in Table 1.

[0081] Example 10 A PBN hearth liner was produced in the same manner as in Example 2, except that the cross section of the main body was processed and polished to have a surface roughness of 1.0 μm on the inner wall surface and 0.5 μm on the outer wall surface. The evaluation results are shown in Table 1.

[0082] Example 11 A PBN hearth liner was produced in the same manner as in Example 2, except that the cross section of the body was processed and polished to have a surface roughness of 5.0 μm on the inner wall surface and 4.5 μm on the outer wall surface. The evaluation results are shown in Table 1.

[0083] Example 12 A PBN hearth liner was produced in the same manner as in Example 2, except that the reaction was carried out using a cylindrical carbon mold 41 with a diameter of 50 mm and an angle θ' (the angle θ' between the plane defining the inner wall surface of the container body and the axis of symmetry of the mold) of 0.5°. The evaluation results are shown in Table 1.

[0084] Example 13 A PBN hearth liner was produced in the same manner as in Example 2, except that the reaction was carried out using a cylindrical carbon mold 41 with a diameter of 50 mm and an angle θ' (the angle θ' between the plane defining the inner wall surface of the container body and the axis of symmetry of the mold) of 60°. The evaluation results are shown in Table 1.

[0085] Example 14 After processing and polishing, the main body 42 was placed back in the CVD furnace, and the temperature was kept at 2000°C. Propane gas, which serves as a carbon source, was introduced at a rate of 3 L / min. The reaction time was adjusted to form a 5 μm-thick PG layer 43 on the surface of the main body 42. A PBN hearth liner was fabricated in the same manner as in Example 2. The evaluation results are shown in Table 1.

[0086] Example 15 After processing and polishing, the main body 42 was placed back in the CVD furnace, and the temperature was kept at 2000°C. Propane gas, which serves as a carbon source, was introduced at a rate of 3 L / min. The reaction time was adjusted to laminate a PG layer 43 having a thickness of 100 μm on the surface of the main body 42. A PBN hearth liner was fabricated in the same manner as in Example 2. The evaluation results are shown in Table 1.

[0087] (Comparative Example 1) A PBN hearth liner was produced in the same manner as in Example 2, except that the cross section of the body was processed and polished so that the R shape of the tip of the inner wall was 0 mm. The evaluation results are shown in Table 1. (Comparative Example 2) The reaction was carried out by changing the diameter to a cylindrical carbon mold 41 with a diameter of 50 mm and a layer cross section angle parallel to the central axis, and the reaction conditions were adjusted to a body density of 1.5 g / cm 3 The cross section of the body was processed and polished so that the R shape of the inner wall tip was 0 mm and the surface roughness of the inner and outer wall surfaces was 0.1 μm, and the reaction time was adjusted to laminate a 2 μm PG layer 43. A PBN hearth liner was produced in the same manner as in Example 2. The evaluation results are shown in Table 1.

[0088] The results of Examples 1 to 15 and Comparative Examples 1 and 2 are summarized in Table 1 below.

[0089] [Table 1]

[0090] From Table 1, it can be seen that the PBN hearth liners of Examples 1 to 15 can be used 105 times or more and have excellent durability. Among them, the PBN hearth liners of Examples 1 to 15 have an angle of 50° between the layer cross section and the inner wall surface in contact with the layer cross section, a tip R shape of 0.5 mm, a length of the flat surface of the tip of 0.2 mm, and a density of 1.9 g / cm 3 The PBN hearth liner of Example 2, which has an inner surface roughness Ra of 2.0 μm, an outer surface roughness Ra of 1.5 μm, an angle θ' (the angle θ' between the plane defining the inner wall surface of the container body and the axis of symmetry of the mold) of 3°, and a PG film thickness of 30 μm, is extremely durable.

[0091] In contrast, the conventional PBN hearth liner (Comparative Example 1), which has a tip radius of 0 mm, could only be used 86 times, indicating poor durability. Furthermore, Comparative Example 2, which had other parameters that were not optimal, could only be used 5 times, indicating poor durability.

[0092] The present specification includes the following aspects. [1]: A PBN container comprising a container body made of a pyrolytic boron nitride laminate and a conductive film covering the surface of the container body, wherein the angle θ formed by the layer cross section of the container body and the inner wall surface or outer wall surface of the container body that is in contact with the layer cross section is 20° or more and 80° or less over the entire circumference of the opening of the container body, and the tip portion of the opening of the container body has a shape in which the radius of curvature R is 0.2 mm or more and 3.0 mm or less over the entire circumference of the opening of the container body. [2]: The PBN container of [1] above, which has a flat surface at the tip of the opening of the container body, and the length of the flat surface in the radial direction of the container body is 0.05 mm or more and 2 mm or less. [3]: The density of the container body is 1.7 g / cm 3 More than 2.2g / cm 3 The PBN container according to [1] or [2] above, which is as follows: [4]: A PBN container according to any one of [1] to [3] above, wherein the surface roughness Ra of the container body is in the range of 0.5 μm to 5.0 μm. [5]: A PBN container according to any one of [1] to [4] above, wherein the surface roughness Ra of the outer wall side of the container body is smaller than the surface roughness Ra of the inner wall side of the container body. [6]: A PBN container according to any one of [1] to [5] above, wherein the angle θ' between the inner wall surface or outer wall surface of the container body and the axis of symmetry of the container body is 0.5° or more and 60° or less. [7]: The PBN container according to any one of [1] to [6] above, wherein the PBN container is a PBN hearth liner for electron beam evaporation. [8]: The PBN container according to any one of [1] to [7] above, wherein the conductive film is pyrolytic graphite. [9]: A PBN container according to any one of [1] to [8] above, wherein the thickness of the conductive film is 5 μm or more and 100 μm or less.

[10] : A method for manufacturing a PBN container, comprising the steps of forming a container body by stacking pyrolytic boron nitride and processing the shape, and stacking a conductive film on the surface of the container body, wherein in the step of forming the container body, the angle θ between the layer cross-section of the container body and the inner wall surface or outer wall surface of the container body that is in contact with the layer cross-section is 20° or more and 80° or less around the entire circumference of the opening of the container body, and the tip portion of the opening of the container body has a shape with a radius of curvature R of 0.2 mm or more and 3.0 mm or less around the entire circumference of the opening of the container body.

[11] : The method for manufacturing a PBN container according to

[10] , wherein the PBN container to be manufactured is a PBN hearth liner for electron beam evaporation.

[12] : The method for producing a PBN container according to

[10] or

[11] , wherein the conductive film is made of pyrolytic graphite.

[0093] The present invention is not limited to the above-described embodiments. The above-described embodiments are merely examples, and anything that has substantially the same configuration as the technical idea described in the claims of the present invention and that exhibits similar effects is included within the technical scope of the present invention. [Explanation of symbols]

[0094] 10, 44, 50...PBN container (hearth liner), 11, 42...container body, 12, 43...Conductive film (PG layer), 13...Layer cross section, 14...inner wall surface, 15...outer wall surface, 16...inner wall surface of container; 17...upper end surface; 18...Tip, 19...Flat surface, 40...PBN layer, 41 heat-resistant substrate (carbon type), 42...main body, 51...hearth, 52...cooling water, 53...evaporation material.

Claims

1. a container body made of a laminate of pyrolytic boron nitride; a conductive film covering the surface of the container body; A PBN container comprising: an angle θ formed between a layer cross section of the container body and an inner wall surface or an outer wall surface of the container body that is in contact with the layer cross section is 20° or more and 80° or less over the entire circumference of the opening of the container body; the tip of the opening of the container body has a shape with a radius of curvature R of 0.2 mm or more and 3.0 mm or less over the entire circumference of the opening of the container body, A PBN container characterized in that the container body has a flat surface at the tip of the opening, and the length of the flat surface in the radial direction of the container body is 0.05 mm or more and 2 mm or less.

2. The density of the container body is 1.7 g / cm ３ Above, 2.2g / cm ３ 2. The PBN container according to claim 1, wherein:

3. 2. The PBN container according to claim 1, wherein the surface roughness Ra of the container body is in the range of 0.5 μm to 5.0 μm.

4. 2. The PBN container according to claim 1, wherein the surface roughness Ra of the outer wall of the container body is smaller than the surface roughness Ra of the inner wall of the container body.

5. 2. The PBN container according to claim 1, wherein an angle θ′ formed between the inner wall surface or the outer wall surface of the container body and the axis of symmetry of the container body is 0.5° or more and 60° or less.

6. 2. The PBN container according to claim 1, wherein the PBN container is a PBN hearth liner for electron beam evaporation.

7. 2. The PBN container of claim 1, wherein the conductive film is pyrolytic graphite.

8. 2. The PBN container according to claim 1, wherein the conductive film has a thickness of 5 μm or more and 100 μm or less.

9. forming a container body by depositing and shaping pyrolytic boron nitride; laminating a conductive film on the surface of the container body; A method for manufacturing a PBN container, comprising: A method for manufacturing a PBN container, characterized in that, in the step of forming the container body, the angle θ between the layer cross-section of the container body and the inner wall surface or outer wall surface of the container body that is tangent to the layer cross-section is 20° or more and 80° or less around the entire circumference of the opening of the container body, the tip of the opening of the container body has a shape with a radius of curvature R of 0.2 mm or more and 3.0 mm or less around the entire circumference of the opening of the container body, the tip of the opening of the container body has a flat surface, and the length of the flat surface in the radial direction of the container body is 0.05 mm or more and 2 mm or less.

10. 10. The method for manufacturing a PBN container according to claim 9, wherein the PBN container to be manufactured is a PBN hearth liner for electron beam evaporation.

11. 10. The method for manufacturing a PBN container according to claim 9, wherein the conductive film is made of pyrolytic graphite.

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