Silicon component and method for manufacturing silicon component

Abstract

This silicon member (10) is provided with a plurality of plate-shaped members (11, 12) comprising a Si-containing material, the plate-shaped members (11, 12) are joined in the thickness direction, a joining layer (20) is formed between the plate-shaped members (11, 12), and the area ratio of the Si phase in the joining layer (20) is 12% or less. Preferably, the aspect ratio of the Si phase in the bonding layer (20) is 3.0 or less.

Description

Technical Field

[0001] The present invention relates to a silicon component used in, for example, a plasma processing apparatus and a method for manufacturing the silicon component.

[0002] This application claims priority based on patent application No. 2022-073579 filed in Japan on April 27, 2022, and its contents are incorporated herein by reference. Background Art

[0003] Conventionally, in plasma processing devices such as plasma etching devices or plasma CVD devices used in semiconductor device manufacturing processes, an electrode plate and a stage connected to a high-frequency power supply are arranged, for example, vertically opposed to each other in a chamber of the various devices, so that a silicon wafer is placed on the stage. In this state, a high-frequency voltage is applied while a gas is passed through a through hole formed in the electrode plate toward the silicon wafer to generate plasma, and etching and other processes are performed on the silicon wafer.

[0004] In the above-mentioned plasma processing apparatus and the like, silicon or silicon components such as silicon nitride and silicon carbide are widely used in order to suppress metal contamination in the chamber.

[0005] For example, as an electrode plate used in a plasma processing apparatus, a silicon member having a structure in which a plurality of vent holes are formed in a silicon plate is used.

[0006] Silicon components placed in a chamber of a plasma processing apparatus or the like gradually wear out as they are used. Therefore, it is required to join the worn silicon component to another silicon component and reuse the obtained silicon joint body as a silicon component.

[0007] For example, Patent Document 1 discloses a silicon electrode plate formed by joining a plurality of plate-shaped electrode members made of silicon in the thickness direction.

[0008] In Patent Document 1, Al foil is sandwiched between plate-like electrode members and heat-treated at 800° C. to form a joint made of an Al—Si eutectic alloy, thereby joining the plate-like electrode members to each other (see paragraphs 0018 to 0026 of Patent Document 1).

[0009] Patent Document 1: Japanese Patent No. 6146840

[0010] However, in the silicon electrode plate described in Patent Document 1, since the joint portion is composed of a eutectic alloy with silicon (e.g., Al-Si eutectic alloy, etc.), a large amount of Si phase exists in the joint portion. When used in a high temperature environment, the Si phase in the joint portion becomes the starting point of damage, and cracks may occur in the joint portion, resulting in insufficient heat resistance. In addition, pores or shrink holes may occur in the joint portion, resulting in a decrease in joint strength. Summary of the invention

[0011] The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a silicon component having sufficiently high bonding strength and excellent heat resistance and capable of being stably used even in a high-temperature environment, and a method for manufacturing the silicon component.

[0012] In order to solve the above-mentioned problems, the silicon component of scheme 1 of the present invention is characterized in that it has a plurality of plate-like components made of Si-containing material, the plate-like components are joined in the thickness direction, a joining layer is formed between the plate-like components, and the area ratio of the Si phase in the joining layer is less than 12%.

[0013] According to the silicon component of the first embodiment of the present invention, since the area ratio of the Si phase formed in the bonding layer between the plate-like components is 12% or less, the formation of a coarse Si phase in the bonding layer can be suppressed, and even when used in a high temperature environment, damage to the bonding layer can be suppressed, thereby having excellent heat resistance. In addition, there are no many shrinkage cavities or voids in the bonding layer, and the bonding strength is excellent.

[0014] A second aspect of the present invention is the silicon component according to the first aspect of the present invention, wherein the aspect ratio of the Si phase in the bonding layer is 3.0 or less.

[0015] According to the silicon component of the second aspect of the present invention, since the aspect ratio of the Si phase in the bonding layer is 3.0 or less, damage to the bonding layer can be suppressed even when used in a high temperature environment, and the heat resistance is particularly excellent.

[0016] A third aspect of the present invention is the silicon component according to the first or second aspect of the present invention, wherein the bonding layer is made of Al or a metal containing Al.

[0017] According to the silicon member of the third aspect of the present invention, since the bonding layer is composed of Al or a metal containing Al, a plurality of plate-like members composed of a material containing Si can be reliably bonded in the thickness direction.

[0018] A fourth aspect of the present invention is the silicon component according to the third aspect of the present invention, wherein the bonding layer is composed of an Al-Si alloy having a Si content in a range of 0.5 mass % to 12.6 mass %.

[0019] According to the silicon component of the fourth aspect of the present invention, since the bonding layer is composed of an Al-Si alloy having a Si content in the range of 0.5 mass % or more and 12.6 mass % or less, a plurality of plate-like components composed of Si-containing materials can be reliably bonded in the thickness direction. Furthermore, since the area ratio of the Si phase in the bonding layer is controlled to be 12% or less, damage to the bonding layer can be suppressed even when used in a high temperature environment, resulting in particularly excellent heat resistance.

[0020] Scheme 5 of the present invention is characterized in that, in the silicon component of Scheme 3 or Scheme 4 of the present invention, when a line analysis is performed along an imaginary line extending in the thickness direction of the silicon component, the number of intersections of the Si peak and the Al peak on the imaginary line in the bonding layer is four or less.

[0021] According to the silicon component of Scheme 5 of the present invention, since the number of intersections of the Si peak and the Al peak on the imaginary line extending in the thickness direction of the silicon component is four or less in the bonding layer when a line analysis is performed along the imaginary line, the number of Si phases present in the bonding layer is small, and damage to the bonding layer can be suppressed even when used in a high-temperature environment, resulting in particularly excellent heat resistance.

[0022] The manufacturing method of the silicon component of scheme 6 of the present invention is characterized in that the manufacturing method is a method for manufacturing any silicon component in schemes 1 to 5 of the present invention, comprising: a stacking step, arranging a bonding material between a plurality of the plate-like components to form a stack of a plurality of the plate-like components and the bonding material; and a pressurizing and heating step, heating the stack to a temperature lower than the liquidus temperature of the bonding material while being pressurized along the stacking direction.

[0023] According to the method for manufacturing a silicon component of the sixth aspect of the present invention, since the bonding material is heated to a temperature lower than the liquidus temperature in the pressurizing and heating steps, the area ratio of the Si phase in the bonding layer can be controlled to be 12% or less. Therefore, the formation of a coarse Si phase in the bonding layer can be suppressed, and a silicon component with excellent heat resistance can be manufactured.

[0024] Furthermore, in the pressurizing and heating steps, almost no liquid phase is generated, so that overflow of the bonding material can be suppressed, and shrinkage cavities or voids are not formed in the bonding layer, thereby improving the bonding strength.

[0025] A seventh aspect of the present invention is a method for producing a silicon component according to the sixth aspect of the present invention, wherein the bonding material is made of Al or a metal containing Al.

[0026] According to the method for manufacturing a silicon member according to claim 7 of the present invention, since the bonding material is made of Al or a metal containing Al, a plurality of plate-like members made of a material containing Si can be bonded reliably.

[0027] The method for manufacturing a silicon component according to claim 8 of the present invention is characterized in that, in the method for manufacturing a silicon component according to claim 7 of the present invention, the bonding material is composed of an Al-Si alloy having a Si content in a range of 0.5 mass % to 12.6 mass %.

[0028] According to the method for manufacturing silicon parts of scheme 8 of the present invention, since the bonding material is composed of an Al-Si alloy having a Si content in the range of greater than 0.5 mass % and less than 12.6 mass %, the diffusion of Si from the plate-like parts to the bonding layer can be suppressed, thereby enabling the area ratio of the Si phase in the bonding layer to be sufficiently reduced.

[0029] The manufacturing method of the silicon component of scheme 9 of the present invention is characterized in that, in any one of the manufacturing methods of the silicon component in schemes 6 to 8 of the present invention, before the stacking process, there is also an Al layer forming process of forming an Al layer on the bonding surface of the plate-like component. In the stacking process, the plurality of plate-like components are arranged in a manner that the Al layers are opposite to each other, and the bonding material is arranged in a manner that is in contact with the opposite Al layers, thereby forming a stack of the plurality of plate-like components and the bonding material.

[0030] According to the method for manufacturing a silicon component of solution 9 of the present invention, since an Al layer is formed on the bonding surface of the plate-like component, a bonding material is arranged in contact with the Al layer to form a laminate, and the laminate is heated to a temperature lower than the liquidus temperature of the bonding material while being pressurized in the stacking direction, the Al layer can suppress the diffusion of Si from the plate-like component to the bonding material. Therefore, the formation of a coarse Si phase in the bonding layer can be suppressed, and a silicon component with excellent heat resistance can be manufactured.

[0031] According to the aspects of the present invention, it is possible to provide a silicon component having sufficiently high bonding strength and excellent heat resistance and capable of being stably used even in a high-temperature environment, and a method for manufacturing the silicon component. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1A This is an explanatory diagram showing an example of a silicon component according to an embodiment of the present invention, and is a perspective view of the silicon component.

[0033] Figure 1B This is an explanatory diagram showing an example of a silicon component according to an embodiment of the present invention, and is an enlarged explanatory diagram of a bonding layer.

[0034] Figure 2It is an explanatory diagram of the boundary points between the Si phase and the Al phase existing on the virtual line extending in the thickness direction of the bonding layer of the silicon component according to one embodiment of the present invention.

[0035] Figure 3 It is a flowchart showing a method for manufacturing a silicon component according to one embodiment of the present invention.

[0036] Figure 4 It is an explanatory diagram showing a method for manufacturing a silicon component according to one embodiment of the present invention.

[0037] Figure 5A This is a photograph of the bonding layer of the silicon component of Example 1 of the present invention, which is a SEM image.

[0038] Figure 5B This is a photograph of the bonding layer of the silicon component of Example 1 of the present invention, which is the mapping result of Al.

[0039] Figure 5C This is a photograph of the bonding layer of the silicon component of Example 1 of the present invention, which is the result of Si mapping.

[0040] Fig. 6A This is a photograph of the bonding layer of the silicon component of Example 6 of the present invention, which is a SEM image.

[0041] Figure 6B This is a photograph of the bonding layer of the silicon component of Example 6 of the present invention, which is the result of line analysis of Al and Si.

[0042] Figure 6C This is a photograph of the bonding layer of the silicon component of Example 6 of the present invention, which is the mapping result of Al.

[0043] Fig.6D This is a photograph of the bonding layer of the silicon component of Example 6 of the present invention, which is the mapping result of Si.

[0044] Fig. 7A This is a photograph of the bonding layer of the silicon component of Comparative Example 1, which is a SEM image.

[0045] Figure 7B This is a photograph of the silicon component bonding layer of Comparative Example 1, which is the result of line analysis of Al and Si.

[0046] Figure 7C This is a photograph of the bonding layer of the silicon component of Comparative Example 1, which is the mapping result of Al.

[0047] Fig.7D This is a photograph of the bonding layer of the silicon component of Comparative Example 1, which is a result of Si mapping.

[0048] Fig. 8AThis is a schematic explanatory diagram of the tensile test in the example, and is a diagram showing a test piece.

[0049] Figure 8B This is a schematic explanatory diagram of a tensile test in an example, and is a diagram showing a test piece and a tensile test jig.

[0050] Figure 8C This is a schematic explanatory diagram of the tensile test in the examples, and is a diagram showing a tensile testing machine. DETAILED DESCRIPTION

[0051] Hereinafter, a silicon component and a method for manufacturing the silicon component according to embodiments of the present invention will be described.

[0052] The silicon component of this embodiment is a silicon component arranged in a chamber of a plasma processing device such as a plasma etching device or a plasma CVD device used in a semiconductor device manufacturing process, and in this embodiment, is a silicon electrode plate having a structure with a plurality of vent holes formed on a silicon plate. That is, in the silicon component of this embodiment, a plurality of silicon electrode plates that are worn out during use are bonded together and used as a regenerated silicon electrode plate.

[0053] like Figure 1A As shown, the silicon member 10 (regenerated silicon electrode plate) of the present embodiment includes a plurality of vent holes 10A penetrating in the thickness direction.

[0054] Moreover, if Figure 1A , Figure 1B As shown, the silicon member 10 of the present embodiment has a structure in which a first plate member 11 and a second plate member 12 are bonded in the thickness direction, and a bonding layer 20 is formed between the first plate member 11 and the second plate member 12 .

[0055] The first plate-shaped member 11 and the second plate-shaped member 12 are made of a Si-containing material such as silicon, silicon nitride, or silicon carbide.

[0056] Furthermore, the area ratio of the Si phase 25 in the bonding layer 20 formed between the first plate-shaped member 11 and the second plate-shaped member 12 is 12% or less.

[0057] The area ratio of the Si phase 25 in the bonding layer 20 is more preferably 10% or less, and more preferably 8% or less. The lower limit of the area ratio of the Si phase 25 in the bonding layer 20 is not particularly limited, but is preferably 0% or more.

[0058] In the present embodiment, the area ratio of the Si phase 25 in the bonding layer 20 is the area ratio in the cross section of the bonding layer 20 along the stacking direction of the silicon member 10 .

[0059] Furthermore, in the present embodiment, the aspect ratio of the Si phase 25 in the bonding layer 20 is preferably 3.0 or less.

[0060] The aspect ratio of the Si phase 25 in the bonding layer 20 is more preferably 2.5 or less. The lower limit of the aspect ratio of the Si phase 25 in the bonding layer 20 is not particularly limited, but is preferably 1.0 or more. The Si phase 25 in the bonding layer 20 is preferably spherical.

[0061] Furthermore, in the present embodiment, the bonding layer 20 is preferably made of Al or a metal containing Al.

[0062] The joining layer 20 is preferably an Al-Si alloy having a Si content in the range of 0.5 mass % to 12.6 mass %. The joining layer 20 is more preferably an Al-Si alloy having a Si content in the range of 0.5 mass % to 8.0 mass %.

[0063] Furthermore, in this embodiment, when the bonding layer 20 is composed of Al or a metal containing Al, Figure 2 As shown, when line analysis is performed along an imaginary line P extending in the thickness direction of the silicon member 10 , the number of intersections of the Si peak and the Al peak on the imaginary line P is preferably four or less in the bonding layer 20 .

[0064] At this time, if Figure 2 As shown, the Si peak indicates the Si phase 25 in the first plate-shaped member 11, the second plate-shaped member 12, and the bonding layer 20. Furthermore, the Al peak indicates the bonding layer 20 composed of Al or a metal containing Al.

[0065] Therefore, the boundary between the first plate-shaped member 11 and the bonding layer 20 and the boundary between the second plate-shaped member 12 and the bonding layer 20 also serve as intersection points of the Si peak and the Al peak in the bonding layer 20 .

[0066] The lower limit of the number of intersections of the Si peak and the Al peak on the virtual line P is not particularly limited, but is preferably two or more.

[0067] Next, refer to Figure 3 and Figure 4 A method for manufacturing the silicon member 10 according to the present embodiment will be described.

[0068] In the method for manufacturing the silicon component 10 of the present embodiment, Figure 3 and Figure 4As shown, it comprises: a surface grinding step S01, grinding the surfaces of the used silicon electrode plates, namely the first plate-shaped part 11 and the second plate-shaped part 12; an Al layer forming step S02, forming an Al layer 21 on the bonding surfaces of the first plate-shaped part 11 and the second plate-shaped part 12 respectively; a stacking step S03, forming a stack of the first plate-shaped part 11, the bonding material 35 and the second plate-shaped part 12; and a pressurizing and heating step S04, heating the stack while being pressurized along the stacking direction.

[0069] Hereinafter, each step of the method for manufacturing the silicon member 10 according to the present embodiment will be described in detail.

[0070] (Surface grinding process S01)

[0071] In this embodiment, if Figure 4 As shown, prepare two used silicon electrode plates.

[0072] Then, the surface (plasma surface) of the silicon electrode plate is ground by a grinder 40. Thus, the first plate member 11 and the second plate member 12 are obtained. In addition, by grinding the plasma surface, the plasma surface side portion of the vent hole that has expanded in diameter due to wear during use can be removed.

[0073] (Al layer forming step S02)

[0074] Next, the Al layer 21 is formed on each of the bonding surfaces of the first plate-shaped member 11 and the second plate-shaped member 12 .

[0075] The method for forming the Al layer 21 is not particularly limited, and various existing methods such as a vapor deposition method and a sputtering method can be appropriately selected. In the present embodiment, the Al layer 21 is formed by a sputtering method using an Al sputtering target.

[0076] The thickness of the Al layer 21 is preferably set within a range of 0.05 μm to 2 μm.

[0077] (Lamination process S03)

[0078] Next, the first plate member 11 and the second plate member 12 are arranged so that their Al layers 21 , 21 face each other, and the bonding material 35 is arranged so as to be in contact with the facing Al layers 21 , 21 , thereby forming a stack of the first plate member 11 , the bonding material 35 , and the second plate member 12 .

[0079] Here, the bonding material 35 is preferably made of Al or a metal containing Al. In the present embodiment, the bonding material 35 is preferably an Al-Si alloy having a Si content in the range of 0.5 mass % or more and 12.6 mass % or less.

[0080] (Pressure and heating process S04)

[0081] Next, the stacked body is heated while being pressurized in the stacking direction, and the first plate-shaped member 11 and the second plate-shaped member 12 are bonded via the bonding layer 20. In addition, the Al layers 21, 21 formed on the bonding surfaces of the first plate-shaped member 11 and the second plate-shaped member 12 are introduced into the bonding layer 20 during heating in the pressurizing and heating step S04.

[0082] Here, in order to control the area ratio of the Si phase in the bonding layer 20 to 12% or less, the holding temperature in the pressurizing and heating step S04 is set lower than the melting point of the Al layer 21 or lower than the liquidus temperature of the bonding material 35 .

[0083] In the present embodiment, when Al or Al-Si alloy having a Si content in the range of 0 mass % or more and 12.6 mass % or less is used as the bonding material 35, the holding temperature is preferably set in the range of 500° C. or more and 650° C. or less. Furthermore, in the present embodiment, when the Al layer 21 formed on the bonding surfaces of the first plate-shaped member 11 and the second plate-shaped member 12 is used for bonding (when the Al layer 21 is used as the bonding material), the holding temperature is preferably set in the range of 500° C. or more and 650° C. or less.

[0084] When an Al-Si alloy having an Al or Si content in the range of 0.5 mass % to 12.6 mass % is used as the bonding material 35, the lower limit of the holding temperature is preferably set to 550° C. or higher, more preferably 580° C. or higher. Furthermore, the upper limit of the holding temperature is preferably set to 640° C. or lower, more preferably 600° C. or lower.

[0085] Furthermore, the holding time in the pressurizing and heating step S04 is preferably in the range of 1 hour to 16 hours.

[0086] The lower limit of the holding time is more preferably 1.5 hours or more, and more preferably 2 hours or more. The upper limit of the holding time is more preferably 8 hours or less, and more preferably 6 hours or less.

[0087] Furthermore, the pressurizing load in the stacking direction in the pressurizing and heating step S04 is preferably in the range of 0.01 MPa to 10 MPa.

[0088] The lower limit of the pressure load in the stacking direction is more preferably 0.03 MPa or more, and more preferably 0.1 MPa or more. The upper limit of the pressure load in the stacking direction is more preferably 8 MPa or less, and more preferably 6 MPa or less.

[0089] Through the above-described various steps, the silicon member 10 (regenerated silicon electrode plate) according to the present embodiment can be manufactured.

[0090] In the silicon component 10 of the present embodiment configured as described above, since the area ratio of the Si phase 25 in the bonding layer 20 formed between the first plate-shaped component 11 and the second plate-shaped component 12 is 12% or less, it is possible to suppress the formation of a coarse Si phase 25 in the bonding layer 20, and even when used in a high-temperature environment, it is possible to suppress damage to the bonding layer 20, thereby achieving excellent heat resistance. In addition, since a large amount of liquid phase is not generated during bonding, there are not many shrinkage cavities or pores in the bonding layer 20, and thus excellent bonding strength.

[0091] In the silicon component 10 of this embodiment, when the aspect ratio of the Si phase 25 in the bonding layer 20 is 3.0 or less, damage to the bonding layer 20 starting from the Si phase 25 can be suppressed even when used in a high temperature environment, and the heat resistance is particularly excellent.

[0092] Furthermore, in the silicon member 10 of the present embodiment, when the bonding layer 20 is made of Al or a metal containing Al, the first plate-shaped member 11 and the second plate-shaped member 12 made of a material containing Si can be reliably bonded in the thickness direction.

[0093] In addition, in the silicon component 10 of the present embodiment, when the bonding layer 20 is composed of an Al-Si alloy having a Si content in the range of greater than 0.5 mass % and less than 12.6 mass %, diffusion of Si from the first plate-shaped component 11 and the second plate-shaped component 12 composed of Si-containing materials to the bonding layer 20 can be suppressed, and the area ratio of the Si phase in the bonding layer 20 can be substantially reduced.

[0094] According to the method for manufacturing the silicon component 10 of the present embodiment, since the temperature is heated to a temperature lower than the liquidus temperature of the bonding material 35 in the pressurizing and heating step S04, a large amount of liquid phase is not generated during bonding, and the area ratio of the Si phase 25 in the bonding layer 20 can be controlled to be 12% or less. Therefore, the formation of a coarse Si phase 25 in the bonding layer 20 can be suppressed, and the silicon component 10 with excellent heat resistance can be manufactured.

[0095] Furthermore, a large amount of liquid phase is not generated in the pressurizing and heating step S04 , so that overflow of the bonding material 35 can be suppressed, and shrinkage cavities or voids are not formed in the bonding layer 20 , thereby improving the bonding strength.

[0096] In the method for manufacturing the silicon member 10 of the present embodiment, when the bonding material 35 is made of Al or a metal containing Al, the first plate-shaped member 11 and the second plate-shaped member 12 made of a material containing Si can be bonded reliably.

[0097] Furthermore, in the manufacturing method of the silicon component 10 of the present embodiment, since the bonding material 35 is composed of an Al-Si alloy having a Si content in the range of greater than 0.5 mass % and less than 12.6 mass %, the diffusion of Si from the first plate-shaped component 11 and the second plate-shaped component 12 to the bonding layer 20 can be fully suppressed, and the area ratio of the Si phase 25 in the bonding layer 20 can be fully reduced.

[0098] In addition, in the manufacturing method of the silicon component 10 of the present embodiment, it is preferable to have an Al layer forming step S02 of forming an Al layer 21 on the bonding surface of the first plate-shaped component 11 and the second plate-shaped component 12 before the lamination step S03. In addition, in the lamination step S03, it is preferable to arrange the first plate-shaped component 11 and the second plate-shaped component 12 in such a manner that the Al layers 21, 21 are opposed to each other, and arrange the bonding material 35 in such a manner that it is in contact with the opposed Al layers 21, 21, so as to form a laminate of the first plate-shaped component 11, the bonding material 35, and the second plate-shaped component 12. In this case, the formation of a coarse Si phase 25 in the bonding layer 20 can be suppressed, so that the silicon component 10 with excellent heat resistance can be manufactured.

[0099] As mentioned above, although embodiment of this invention was described, this invention is not limited to this, It can change suitably within the range which does not deviate from the technical requirement of this invention.

[0100] For example, in this embodiment, the silicon component is described as a regenerated silicon electrode plate formed by joining two used silicon electrode plates, but it is not limited to this. The silicon component can be any silicon component formed by joining plate-like components made of Si-containing material to each other, or it can be a silicon component formed by joining three or more plate-like components.

[0101] When the silicon member includes three or more plate-like members, the number of intersections of the Si peak and the Al peak on the imaginary line extending in the thickness direction is the number measured within the range of two plate-like members and one bonding layer formed therebetween.

[0102] Furthermore, in the present embodiment, an Al layer is formed on the joining surfaces of the first plate-shaped member and the second plate-shaped member and the joining is performed by a joining material. However, the present invention is not limited to this. An Al layer may not be formed on the joining surfaces, and a joining material may be provided between the first plate-shaped member and the second plate-shaped member for joining.

[0103] Example

[0104] Hereinafter, the results of a confirmation experiment conducted to confirm the effectiveness of the present invention will be described.

[0105] A plate-like member made of silicon (diameter (φ) 125 mm×thickness (t) 5 mm) was prepared. In addition, in Examples 1 to 3, 6, and 7 of the present invention, an Al layer (underlying Al layer) was sputtered onto the bonding surface of the plate-like member using an Al sputtering target as shown in Table 1. In addition, bonding materials shown in Table 1 were prepared.

[0106] A laminated body was formed by laminating the prepared plate-like member, the bonding material, and the plate-like member. The laminated body was pressed and heated under the conditions shown in Table 1 to bond the two plate-like members, thereby manufacturing various silicon members having a bonding layer.

[0107] The obtained silicon components were evaluated as follows. The evaluation results are shown in Table 2.

[0108] (Area ratio of Si phase)

[0109] Using a SEM-EDS device (a scanning electron microscope equipped with an energy dispersive X-ray analyzer), the cross section of the silicon component along the stacking direction was observed, and the Si and the elements constituting the bonding layer (hereinafter referred to as the bonding layer elements) were mapped and analyzed for the bonding layer in the cross section with a field of view of 5000 times. For each mapping result, the quantitative mapping function of the attached software of the SEM-EDS device was used to perform a semi-quantitative calculation for each pixel assuming that only Si and bonding layer elements existed, and a quantitative map showing the content (weight %) of each pixel was prepared. According to the quantitative map prepared, the phase with a Si content of 99% or more in the bonding layer within the field of view was set as the Si phase, and the area ratio of the Si phase in the bonding layer within the field of view was calculated.

[0110] The area ratio of the Si phase within the outline of the bonding layer in the field of view is calculated. The field of view used for calculation is multiple and three fields of view (three images), and the area ratio is their average value. In addition, the observation magnification is selected as long as the magnification that can make the upper and lower interfaces of the bonding layer enter the field of view.

[0111] Here, the observation results (cross-sectional structure of SEM) and mapping results of Example 1 of the present invention are shown in Figure 5A to Figure 5C The observation results (cross-sectional structure of SEM), line analysis results of elements, and mapping results of Example 6 of the present invention are shown in Figure 6A to Figure 6D The observation results (cross-sectional structure of SEM), line analysis results of elements, and mapping results of Comparative Example 1 are shown in Figure 7A to Figure 7D middle.

[0112] (Aspect ratio of Si phase)

[0113] The aspect ratios of the Si phases obtained above were calculated using commercially available image analysis software (WIN Roof), and the average value thereof was obtained.

[0114] The longest dimension of the observed Si phase was defined as the major axis length, the longest dimension in a direction perpendicular to the major axis was defined as the minor axis length, and the aspect ratio was defined as major axis length / minor axis length.

[0115] (Number of intersections between Al peak and Si peak)

[0116] The cross section of the obtained silicon component along the stacking direction was observed, and the bonding layer in the cross section was subjected to SEM-EDS analysis (element line analysis). An imaginary line extending in the thickness direction of the bonding layer was drawn on the cross section including the bonding layer, and the number of intersections of the Al peak and the Si peak on the extended imaginary line was counted. In addition, the SEM-EDS line analysis results of Example 6 of the present invention and Comparative Example 1 are shown in FIG. Figure 6B and Figure 7B middle.

[0117] (Appearance Observation)

[0118] Visually observe the appearance of the obtained silicon parts, and evaluate whether the bonding material has overflow and cracks. The situation where the bonding material overflows and cracks are confirmed is marked as "D" (poor). The situation where the bonding material overflows, but there is no crack is marked as "C" (general). The situation where the bonding material overflows and cracks are not confirmed is marked as "B" (good).

[0119] (Joint strength)

[0120] like Figure 8A to Figure 8C As shown in the figure, the obtained silicon component was cut into 10 mm squares, and the surface of the plate-like component opposite to the bonding surface was bonded to the tensile test fixture using an adhesive. Then, it was set on a universal tensile tester and a tensile test was performed at a speed of 0.1 mm / min. In addition, when the bonding strength between the plate-like component bonded with an adhesive and the tensile test fixture exceeded 15 MPa, it was marked as "15 MPa or more".

[0121] (Heat resistance test)

[0122] The obtained silicon parts were kept at 300°C for 24 hours, and then their appearance was visually observed to confirm the presence of cracks or peeling. In addition, for silicon parts where no cracks or peeling were observed visually, ultrasonic flaw detection was implemented before and after heating at 300°C. After confirmation, the case where cracks or peeling were confirmed was marked as "D" (poor). In the silicon parts where no cracks or peeling were confirmed, the case where the ultrasonic flaw detection image changed (the bonding rate changed) was marked as "B" (good). The case where there was no change in the ultrasonic flaw detection image (the bonding rate changed) was marked as "A" (excellent).

[0123] [Table 1]

[0124]

[0125] [Table 2]

[0126]

[0127] In Comparative Example 1, no Al layer was formed on the bonding surface of the plate-like component, Al was used as the bonding material, and bonding was performed without pressurization and at a temperature of 800°C. As a result, the area ratio of the Si phase in the bonding layer was 13%, and the aspect ratio of the Si phase was 4.5. In addition, the number of intersections between the Al peak and the Si peak was 10, and the number of Si phases present in the bonding layer increased. Moreover, the bonding strength was as low as 4.1 MPa, and cracks or peeling were confirmed after the heat resistance test. In addition, overflow of the bonding material was confirmed in the obtained silicon component.

[0128] In Comparative Example 2, no Al layer was formed on the bonding surface of the plate-like component, Al was used as the bonding material, and bonding was performed under the conditions of a pressure load of 3 MPa and a temperature of 800°C. As a result, the area ratio of the Si phase in the bonding layer was 14%, and the aspect ratio of the Si phase was 4.3. In addition, the number of intersections between the Al peak and the Si peak was 12, and the number of Si phases present in the bonding layer increased. The bonding strength was as low as 5.3 MPa, and cracking or peeling was confirmed after the heat resistance test. In addition, overflow and cracking of the bonding material were confirmed in the obtained silicon component.

[0129] In Comparative Example 3, no Al layer was formed on the bonding surface of the plate-like components, Al was used as the bonding material, and bonding was attempted under the conditions of a pressure load of 3 MPa and a holding temperature of 600° C. However, the plate-like components could not be bonded to each other, and a silicon component could not be obtained.

[0130] In contrast, in Example 1 of the present invention, an Al layer was formed on the bonding surface of the plate-like component, Al was used as the bonding material, and bonding was performed under the conditions of a pressure load of 3 MPa and a temperature of 600°C. As a result, the area ratio of the Si phase in the bonding layer was 0%, the number of intersections between the Al peak and the Si peak was two, and there was no Si phase in the bonding layer. Moreover, the bonding strength was as high as 15 MPa or more, and no cracks or peeling were confirmed after the heat resistance test. Furthermore, no overflow of the bonding material was confirmed in the obtained silicon component. In addition, as Figure 5A to Figure 5C As shown in FIG. 1 , it was confirmed that there was no Si phase in the bonding layer. It is presumed that the diffusion of Si from the plate-like member to the bonding layer was suppressed by the Al layer.

[0131] In Example 2 of the present invention, an Al layer was formed on the bonding surface of the plate-like component, Al was used as a bonding material, and bonding was performed under the conditions of a pressure load of 3 MPa and a temperature of 550°C. As a result, the area ratio of the Si phase in the bonding layer was 0%, the number of intersections between the Al peak and the Si peak was two, and there was no Si phase in the bonding layer. Moreover, the bonding strength was as high as 15 MPa or more, and no cracks or peeling were confirmed after the heat resistance test, and no changes in the ultrasonic flaw detection image (changes in the bonding rate) were observed. In addition, no overflow of the bonding material was confirmed in the obtained silicon component.

[0132] In Example 3 of the present invention, an Al layer was formed on the bonding surface of the plate-like component, an Al-7.5 mass% Si alloy was used as a bonding material, and bonding was performed under the conditions of a pressurized load of 3 MPa and a temperature of 600°C. As a result, the area ratio of the Si phase in the bonding layer was 7.8%, and the aspect ratio of the Si phase was 2.2. In addition, the number of intersections of the Al peak and the Si peak was eight. Moreover, the bonding strength was as high as 15 MPa or more, and no cracks or peeling were confirmed after the heat resistance test, and no changes in the ultrasonic flaw detection image (changes in the bonding rate) were observed. In addition, no overflow of the bonding material was confirmed in the obtained silicon component.

[0133] In Example 4 of the present invention, an Al layer is not formed on the bonding surface of the plate-like component, an Al-7.5 mass% Si alloy is used as a bonding material, and bonding is performed under the conditions of a pressurized load of 3 MPa and a temperature of 600°C. As a result, the area ratio of the Si phase in the bonding layer is 8.0%, and the aspect ratio of the Si phase is 2.9. In addition, the number of intersections of the Al peak and the Si peak is six. In addition, the bonding strength is relatively high, at 14.1 MPa, and no cracking or peeling is confirmed after the heat resistance test. In addition, no overflow of the bonding material is confirmed in the obtained silicon component. In addition, although there is a small amount of Si phase in the bonding layer, it is confirmed that the aspect ratio of the Si phase is small enough.

[0134] In Example 5 of the present invention, an Al layer was not formed on the bonding surface of the plate-like component, an Al-2.0 mass% Si alloy was used as a bonding material, and bonding was performed under the conditions of a pressurized load of 3 MPa and a temperature of 600°C. As a result, the area ratio of the Si phase in the bonding layer was 2.4%, and the aspect ratio of the Si phase was 2.4. In addition, the number of intersections of the Al peak and the Si peak was four. Moreover, the bonding strength was as high as 15 MPa or more, and no cracks or peeling were confirmed after the heat resistance test, and no changes in the ultrasonic flaw detection image (changes in the bonding rate) were observed. In addition, no overflow of the bonding material was confirmed in the obtained silicon component.

[0135] In Example 6 of the present invention, an Al layer was formed on the bonding surface of the plate-like component without using a bonding material, and bonding was performed under the conditions of a pressure load of 3 MPa and a temperature of 600°C. As a result, the area ratio of the Si phase in the bonding layer was 0%, the number of intersections between the Al peak and the Si peak was two, and there was no Si phase in the bonding layer. Moreover, the bonding strength was as high as over 15 MPa, no cracking or peeling was confirmed after the heat resistance test, and no changes in the ultrasonic flaw detection image (changes in the bonding rate) were observed. Furthermore, no overflow of the bonding material was confirmed in the obtained silicon component. In addition, as Figure 6A to Figure 6D As shown, it was confirmed that no Si phase existed in the bonding layer.

[0136] In Example 7 of the present invention, an Al layer was formed on the bonding surface of the plate-like component, pure Al was used as the bonding material, and bonding was performed under the conditions of a pressure load of 3 MPa and a temperature of 600°C. As a result, the area ratio of the Si phase in the bonding layer was 0%, the number of intersections between the Al peak and the Si peak was two, and there was no Si phase in the bonding layer. Moreover, the bonding strength was as high as 15 MPa or more, and no cracks or peeling were confirmed after the heat resistance test, and no changes in the ultrasonic flaw detection image (changes in the bonding rate) were observed. In addition, no overflow of the bonding material was confirmed in the obtained silicon component.

[0137] From the above results, it was confirmed that according to the present example, a silicon component having sufficiently high bonding strength and excellent heat resistance and capable of being stably used even in a high-temperature environment and a method for manufacturing the silicon component can be provided.

[0138] Industrial Applicability

[0139] The silicon member of the present embodiment is suitable as an electrode plate used in a plasma processing apparatus such as a plasma etching apparatus or a plasma CVD apparatus.

[0140] Explanation of symbols

[0141] 10 Silicon parts (recycled silicon electrode plates)

[0142] 11 first plate-shaped member

[0143] 12 second plate-shaped member

[0144] 20 bonding layer

[0145] 21Al layer

[0146] 25Si phase

Claims

1. A silicon component, characterized in that: A plurality of plate-like members made of a Si-containing material are provided, wherein the plate-like members are joined in a thickness direction. A bonding layer is formed between the plate-like members, and an area ratio of a Si phase in the bonding layer is 12% or less.

2. The silicon component according to claim 1, characterized in that The aspect ratio of the Si phase in the bonding layer is 3.0 or less.

3. The silicon component according to claim 1, characterized in that The bonding layer is composed of Al or a metal containing Al.

4. The silicon component according to claim 3, characterized in that The bonding layer is composed of an Al-Si alloy having a Si content in a range of 0.5 mass % to 12.6 mass %.

5. The silicon component according to claim 3, characterized in that When a line analysis is performed along an imaginary line extending in the thickness direction of the silicon member, the number of intersection points between a Si peak and an Al peak on the imaginary line is four or less in the bonding layer.

6. A method for manufacturing a silicon component, characterized in that: The manufacturing method is a method for manufacturing a silicon component according to any one of claims 1 to 5, comprising: a lamination step of disposing a bonding material between the plurality of plate-like members to form a laminate of the plurality of plate-like members and the bonding material; and The pressurizing and heating step heats the stacked body to a temperature lower than the liquidus temperature of the bonding material while being pressurized in the stacking direction.

7. The method for manufacturing a silicon component according to claim 6, characterized in that: The bonding material is made of Al or a metal containing Al.

8. The method for manufacturing a silicon component according to claim 7, characterized in that: The bonding material is composed of an Al-Si alloy having a Si content in a range of 0.5 mass % or more and 12.6 mass % or less.

9. The method for manufacturing a silicon component according to claim 6, characterized in that: Prior to the lamination step, an Al layer forming step of forming an Al layer on the bonding surface of the plate-like member is further included. In the lamination step, the plurality of plate-like members are arranged so that the Al layers thereof face each other, and a bonding material is arranged so as to be in contact with the facing Al layers, thereby forming a laminate of the plurality of plate-like members and the bonding material.

Images