Thermal-sprayed film coated member and method for manufacturing the same
The development of a sprayed film-coated member with a continuous insulating ceramic sprayed film addresses the issue of insufficient insulation in semiconductor manufacturing equipment, effectively suppressing creeping discharge and enhancing insulation performance.
Patent Information
- Application Number
- JP2023193825
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2023-11-14
- Publication Date
- 2025-05-26
AI Technical Summary
Existing joined bodies used in semiconductor manufacturing equipment face issues with insufficient electrical insulation, leading to creeping discharge when the metal base or joining interface is exposed.
A sprayed film-coated member is developed with a continuous insulating ceramic sprayed film applied to specific surfaces of the metal base, the joining interface, and the ceramic sintered body base material, with a porosity of 0.5% to 7% and a thickness of 50 μm or more, to enhance insulation and prevent creeping discharge.
The solution effectively improves the insulation performance of the joined body, suppresses creeping discharge, and enhances the withstand voltage characteristics, making it suitable for use in semiconductor manufacturing equipment.
Smart Images

Figure 2025080576000001_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a thermal spray film-coated member and a method for manufacturing the same.
Background Art
[0002] A joined body obtained by joining a ceramic sintered body substrate and a metal base has been used for various applications as a member for semiconductor manufacturing equipment. For example, a joined body obtained by joining an AlN substrate and a metal base may be used as a semiconductor manufacturing member using high frequency. At that time, in order to prevent creeping discharge from the metal base to the substrate to be processed and the surrounding conductor members, an insulating ceramic thermal spray film made of Al 2 O 3 or the like may be formed. Conventionally, for example, as shown in FIG. 9, an insulating ceramic thermal spray film was formed only on the side surface of the metal base, and no insulating film was formed on the side surface of the AlN substrate. FIG. 9 is a schematic partial cross-sectional view showing an example of a member in which an insulating ceramic thermal spray film is formed on a conventional joined body.
[0003] In a member in which an insulating film is formed on the metal base of such a joined body, if the metal base or the joining interface between the ceramic sintered body substrate and the metal base is exposed, electrical insulation becomes insufficient and creeping discharge may occur.
[0004] Patent Document 1 discloses a thermal spray member in which a thermal spray film made of yttrium oxide (Y 2 O 3 ) adheres to the surface of a substrate made of aluminum or an aluminum alloy, wherein the pores of the thermal spray film are 2% or less, and the adhesion strength between the substrate and the thermal spray film is 20 MPa or more.
[0005] Patent Document 2 discloses a thermal spray member including a substrate made of aluminum and a thermal spray film made of yttrium-containing zirconia, wherein, in a cross-section of a plane orthogonal to the interface between the sprayed surface of the substrate and the thermal spray film, the distance between two parallel straight lines sandwiching the interface is 0.2 μm or less over a length of 10 μm or more.
Prior Art Documents
Patent Documents
[0006]
Patent Document 1
Patent Document 2
Summary of the Invention
Problems to be Solved by the Invention
[0007] Patent Document 1 and Patent Document 2 improve the functionality of metal members by forming an insulating sprayed film on the surface of the metal members. However, Patent Document 1 and Patent Document 2 do not pay attention to the fact that there is a risk of creeping discharge when an insulating sprayed film is formed on the metal base of the joined body.
[0008] The present invention has been made in view of such circumstances, and an object thereof is to provide a sprayed film - coated member that can improve the insulation performance of a joined body and suppress creeping discharge, and a method for manufacturing the sprayed film - coated member.
Means for Solving the Problems
[0009] (1) To achieve the above object, the sprayed film - coated member of the present invention takes the following means. That is, the sprayed film - coated member of an application example of the present invention is a sprayed film - coated member, comprising a ceramic sintered body base material, a metal base joined to the ceramic sintered body base material, an insulating ceramic sprayed film continuously formed on a specific surface of the metal base, a surface of a joining interface between the ceramic sintered body base material and the metal base, and a surface of the ceramic sintered body base material in the vicinity of the surface of the joining interface.
[0010] Thus, by continuously forming an insulating ceramic sprayed film on a specific surface of the metal base, a surface of the bonding interface between the ceramic sintered body base material and the metal base, and a surface of the ceramic sintered body base material near the surface of the bonding interface, slight exposure of the metal base and exposure of the bonding interface can be prevented, and when the sprayed film-coated member is used as a member for a semiconductor manufacturing apparatus, creeping discharge can be suppressed.
[0011] (2) Further, in the sprayed film-coated member of the application example of (1) above, the insulating ceramic sprayed film is characterized in that the porosity is 0.5% or more and 7% or less.
[0012] Thereby, a dense insulating ceramic sprayed film can be formed, and the withstand voltage characteristics of the sprayed film-coated member can be further improved. As a result, creeping discharge can be more suppressed.
[0013] (3) Further, in the sprayed film-coated member of the application example of (1) or (2) above, the insulating ceramic sprayed film is characterized in that it has a two-layer structure with different microstructures.
[0014] Thereby, the thickness of the insulating ceramic sprayed film can be increased, and the withstand voltage characteristics of the insulating ceramic sprayed film can be improved. As a result, creeping discharge can be more suppressed.
[0015] (4) Further, in the sprayed film-coated member of any one of the application examples of (1) to (3) above, the thickness of the insulating ceramic sprayed film in the direction perpendicular to the specific surface of the metal base is characterized in that it is 50 μm or more.
[0016] Thereby, sufficient withstand voltage characteristics can be obtained, and creeping discharge can be more suppressed.
[0017] (5) Further, in the sprayed film-coated member of the application example of (1) or (2) above, the space volume Vvv (μm 3 / μm 2) and 0.001 ≦ (Vvv / (D50) 3 ) ≦ 0.40, where Vvv is the space volume (μm
[0018] This makes it easier for the ceramic sintered body substrate and the insulating ceramic sprayed film to adhere, and improves the durability of the sprayed film coating member. Also, AlN or Al 2 O 3 which is difficult to adhere to the insulating ceramic sprayed film, can be used as the material of the ceramic sintered body substrate, expanding the applications of the sprayed film coating member.
[0019] (6) Also, in the sprayed film coating member of the application example of (3) above, with respect to the space volume Vvv (μm 3 / μm 2 ) of the sprayed surface of the ceramic sintered body substrate and the average particle diameter D50 (μm) of the ceramic raw material for forming the insulating ceramic sprayed film on the ceramic sintered body substrate side, 0.001 ≦ (Vvv / (D50) 3 ) ≦ 0.40 is satisfied.
[0020] This makes it easier for the ceramic sintered body substrate and the insulating ceramic sprayed film to adhere, and improves the durability of the sprayed film coating member. Also, AlN or Al 2 O 3 which is difficult to adhere to the insulating ceramic sprayed film, can be used as the material of the ceramic sintered body substrate, expanding the applications of the sprayed film coating member.
[0021] (7) Also, the manufacturing method of the sprayed film covering member of the application example of the present invention is a manufacturing method of a sprayed film covering member, wherein the space volume Vvv (μm 3 / μm 2A first adjustment step of adjusting to a predetermined range, a second adjustment step of adjusting the surface roughness Sa (μm) of the sprayed surface of the metal base to a predetermined range, a joining step of joining the ceramic sintered body base material and the metal base, and the sprayed surface of the ceramic sintered body base material, the surface of the joining interface between the ceramic sintered body base material and the metal base, and the sprayed surface of the metal base, a coating step of forming an insulating ceramic sprayed film by plasma spraying a slurry composed of water and an insulating ceramic raw material powder having an average particle diameter D50 in the range of 0.5 μm or more and 10 μm or less, wherein the first adjustment step is such that 0.001 ≦ (Vvv / (D50) 3 ) ≦ 0.40.
[0022] Thereby, the ceramic sintered body base material and the insulating ceramic sprayed film are likely to adhere to each other, surface discharge can be suppressed, and a sprayed film coating member excellent in durability can be manufactured. Further, a sprayed film coating member using AlN or Al 2 O 3 as a material of the ceramic sintered body base material can be manufactured.
[0023] (8) Further, the method for manufacturing a sprayed film coating member according to an application example of the present invention is a method for manufacturing a sprayed film coating member, which includes a space volume Vvv (μm 3 / μm 2A first adjustment step of adjusting to a predetermined range, a second adjustment step of adjusting the surface roughness Sa (μm) of the sprayed surface of the metal base to a predetermined range, a joining step of joining the ceramic sintered body base material and the metal base material, and the sprayed surface of the ceramic sintered body base material, the surface of the joining interface between the ceramic sintered body base material and the metal base material, and the sprayed surface of the metal base, a first coating step of forming a first insulating ceramic sprayed film by plasma spraying a first slurry composed of water and a first insulating ceramic raw material powder having an average particle diameter D50 in the range of 0.5 μm or more and 10 μm or less, and a second coating step of spraying a second insulating ceramic raw material powder on the surface of the first insulating ceramic sprayed film to form a second insulating ceramic sprayed film, wherein the first adjustment step adjusts and the average particle diameter D50 such that 0.001 ≦ (Vvv / (D50) 3 ) ≦ 0.40.
[0024] As a result, the ceramic sintered body base material and the insulating ceramic sprayed film are likely to adhere to each other, surface discharge can be suppressed, and a sprayed film coating member excellent in durability can be manufactured. Further, the insulating ceramic sprayed film can be thickened, and the withstand voltage characteristics can be improved. Further, a sprayed film coating member using AlN or Al 2 O 3 as the material of the ceramic sintered body base material can be manufactured.
Advantages of the Invention
[0025] According to the present invention, a sprayed film coating member with improved insulation performance and suppressed surface discharge can be obtained. Further, such a sprayed film coating member can be manufactured.
Brief Description of the Drawings
[0026]
Figure 1
Figure 2
Figure 3
Figure 4
Figure 5
Figure 6
Figure 7
Figure 8
Figure 9
Embodiments for Carrying Out the Invention
[0027] Next, embodiments of the present invention will be described with reference to the drawings. For ease of understanding of the description, the same reference numerals are assigned to the same components in each drawing, and overlapping descriptions are omitted. In the configuration diagrams, the sizes of the respective components are conceptually represented and do not necessarily represent actual dimensional ratios.
[0028] [First Embodiment] (Configuration of Thermal Spray Film Coating Member) The thermal spray film coating member according to the first embodiment of the present invention will be described with reference to FIGS. 1 to 4. FIGS. 1 and 2 are schematic perspective views showing an example of the thermal spray film coating member according to the first embodiment of the present invention. FIGS. 3 and 4 are schematic partial cross-sectional views showing an example of the thermal spray film coating member according to the first embodiment of the present invention. The thermal spray film coating member 100 according to the present embodiment includes a ceramic sintered body base material 110, a metal base 120, and an insulating ceramic thermal spray film 140.
[0029] The shape of the thermal spray film coating member 100 is selected according to its use and the configuration of a semiconductor manufacturing apparatus or the like in which it is installed. For example, the whole may be cylindrical or prismatic, or it may have a stepped shape in which a cylindrical or prismatic ceramic sintered body base material 110 is joined to a cylindrical or prismatic metal base 120 having a different diameter or side length. The size of the thermal spray film coating member 100 is selected according to its use and the configuration of a semiconductor manufacturing apparatus or the like in which it is installed. For example, when the thermal spray film coating member 100 is cylindrical, it can be made into a large member having a diameter of φ300 to 360 mm and a thickness of about 10 to 80 mm. This is because the insulating ceramic thermal spray film 140 of the present invention has a high adhesive strength with the ceramic sintered body base material 110 and the metal base 120.
[0030] The ceramic sintered body base material 110 is made of a ceramic sintered body. The material of the ceramic sintered body base material 110 can be selected from various materials. For example, non-oxidizing ceramics such as AlN sintered body, SiC sintered body, Si 3 N 4 sintered body, and oxides such as Al 2 O 3 sintered body, Y 2 O 3 sintered body, and complex oxides such as YAG (Y 3 Al 5 O 12 ) can be used. The ceramic sintered body base material 110 may be formed of an AlN sintered body, a SiC sintered body, or an Al 2 O 3 sintered body. The ceramic sintered body base material 110 may be formed of an AlN sintered body, a SiC sintered body, or an Al 2 O 3The sintered body is a brittle material and has poor adhesion with other ceramic materials. However, the spraying method of the present invention can form an insulating ceramic sprayed film 140 while reducing the risk of strength reduction or substrate breakage of the substrate material even for such a material, and can improve the insulation performance of the sprayed film covering member 100.
[0031] The metal base 120 is made of metal. The material of the metal base 120 can be selected from various ones. For example, metals such as Mo, Al alloys (5052, 6061), SUS304, and Ti can be used. The metal base 120 is joined to the ceramic sintered body substrate 110. A member in which the ceramic sintered body substrate 110 and the metal base 120 are joined is called a joined body 130.
[0032] The joining of the ceramic sintered body substrate 110 and the metal base 120 can be selected from various joining methods. For example, direct joining without using a joining material, Al joining using a joining material (a method of fusing with an Al foil sandwiched between the ceramic sintered body substrate 110 and the metal base 120), Au joining (similarly, a method of fusing with an Au foil sandwiched), In joining (similarly, a method of fusing with an In foil sandwiched), organic adhesion (a method of adhering with an organic adhesive containing a resin such as silicone), etc. can be selected. When using a joining material, its thickness is preferably 100 μm or less.
[0033] It is preferable that no joining material is confirmed at the joining interface 150. Therefore, the joining method is preferably direct joining that can make the joining layer (a layer different from the ceramic sintered body substrate 110 and the metal base 120) at the joining interface 150 sufficiently thin. By making the joining layer sufficiently thin, the insulation can be improved even when the thickness of the insulating ceramic sprayed film 140 is thin. Also, the sprayed film covering member 100 joined by direct joining is suitable for high-temperature applications. Note that even in the case of direct joining, a joining layer may be formed due to the chemical reaction between the metal base 120 and the ceramic sintered body substrate 110, but its thickness is sufficiently thin.
[0034] The insulating ceramic sprayed film 140 is continuously formed on a specific surface 122 of the metal base 120, a surface 152 of the bonding interface between the ceramic sintered body base material 110 and the metal base 120, and a surface 112 of the ceramic sintered body base material near the surface 152 of the bonding interface. Thereby, the creeping discharge of the sprayed film coating member 100 is suppressed and the insulation performance is improved. As a result, the sprayed film coating member 100 can be applied to various uses.
[0035] The specific surface 122 of the metal base 120 is a surface of the metal base 120 that needs to prevent creeping discharge in the environment where the sprayed film coating member 100 is used. For example, among the surfaces of the metal base 120, the surface that is exposed to the space where plasma is generated in the chamber where the sprayed film coating member 100 is installed is the specific surface 122 of the metal base 120. Therefore, depending on the use of the sprayed film coating member 100 and the shape of the metal base 120, the specific surface 122 of the metal base 120 may be a part of the surface of the metal base 120 or may be the entire surface of the metal base 120.
[0036] The surface 152 of the bonding interface between the ceramic sintered body base material 110 and the metal base 120 is a part adjacent to the specific surface 122 of the metal base 120 among the exposed portions of the bonding interface 150 between the ceramic sintered body base material 110 and the metal base 120. Therefore, even for the exposed portion of the bonding interface 150, the portion not adjacent to the specific surface 122 of the metal base 120 does not have to be coated with the insulating ceramic sprayed film 140. This is because even for the exposed portion of the bonding interface 150, the portion not adjacent to the specific surface 122 of the metal base 120 is not related to creeping discharge.
[0037] The surface 112 of the ceramic sintered body substrate near the surface 152 of the bonding interface refers to the surface 112 of the ceramic sintered body substrate adjacent to the surface 152 of the bonding interface, within a range where it is necessary to coat with the insulating ceramic sprayed film 140 to suppress the creeping discharge of the sprayed film covering member 100 and improve the insulation performance. Therefore, the surface 112 of the ceramic sintered body substrate near the surface 152 of the bonding interface preferably includes at least within 1 mm from the surface 152 of the bonding interface. Also, when the sprayed film covering member 100 has a cylindrical, prismatic, or stepped shape of these, the entire side surface thereof may be coated with the insulating ceramic sprayed film 140. Thereby, even when the adhesion between the ceramic sintered body substrate 110 and the insulating ceramic sprayed film 140 is not good, the creeping discharge of the sprayed film covering member 100 can be sufficiently suppressed, and the manufacturing process becomes simple.
[0038] The insulating ceramic sprayed film 140 is a sprayed film made of insulating ceramic. The insulating ceramic sprayed film 140 can be selected from various materials. For example, Al 2 O 3 (alumina), Y 2 O 3 (yttria), YAG (Y 3 Al 5 O 12 : yttrium aluminum garnet), TiO 2 (titania), Cr 2 O 3 (chromia), silicon nitride (Si 3 N 4 ), aluminum nitride (AlN), and other insulating ceramics can be used. The insulating ceramic sprayed film 140 may be composed of two or more combinations. Composed of two or more combinations means that the insulating ceramic sprayed film 140 is formed by a mixture of particles made of different raw materials.
[0039] The insulating ceramic sprayed film 140 preferably has a porosity of 0.5% or more and 7% or less, more preferably 0.5% or more and 4% or less, and even more preferably 0.5% or more and 3% or less. Thereby, a dense insulating ceramic sprayed film 140 can be formed, and the withstand voltage characteristics of the sprayed film coating member 100 can be further improved. As a result, creepage discharge can be further suppressed. The porosity of the insulating ceramic sprayed film 140 can be confirmed by a SEM image 1000 times the cross-section of the insulating ceramic sprayed film 140.
[0040] The thickness in the direction perpendicular to the specific surface 122 of the metal base 120 of the insulating ceramic sprayed film 140 is preferably 50 μm or more. Thereby, sufficient withstand voltage characteristics can be obtained and creepage discharge can be suppressed. The upper limit of the thickness in the direction perpendicular to the specific surface 122 of the metal base 120 of the insulating ceramic sprayed film 140 does not particularly need to be defined, but can be, for example, 100 μm or less.
[0041] The space volume Vvv (μm 3 / μm 2 ) of the sprayed surface (the surface 112 of the ceramic sintered body base material near the surface 152 of the bonding interface) of the ceramic sintered body base material 110, and the average particle diameter D50 (μm) of the ceramic raw material forming the insulating ceramic sprayed film 140 preferably satisfy 0.001 ≦ (Vvv / (D50) 3 ) ≦ 0.40.
[0042] The space volume Vvv (μm 3 / μm 2 ) of the sprayed surface of the ceramic sintered body base material 110 can be measured using a coherence correlation interferometer. The space volume Vvv (μm 3 / μm 2 ) of the sprayed surface in this specification is a value measured with a load area ratio of 80%. Also, the average particle diameter D50 (μm) of the ceramic raw material forming the insulating ceramic sprayed film 140 can be measured by a particle size measuring device using the laser diffraction / scattering method.
[0043] When the thickness of the insulating ceramic sprayed film 140 is D and the thickness of the bonding layer at the bonding interface 150 is G, it is preferable that D > G. When the bonding layer has a certain thickness, by making the insulating ceramic sprayed film 140 thicker than that, the insulation can be further enhanced.
[0044] It is preferable that there is no chemical bond between the elements constituting the ceramic sintered body substrate 110 and the insulating ceramic sprayed film 140. The absence of a chemical bond between the elements constituting the ceramic sintered body substrate 110 and the insulating ceramic sprayed film 140 means a state in which the insulating ceramic sprayed film 140 and the ceramic sintered body substrate 110 are physically adhered due to the so-called anchor effect. That is, the molten sprayed particles enter the fine valleys present in the ceramic sintered body substrate 110, and the sprayed particles solidify in these valleys. Then, the cooled and solidified sprayed particles exert a compressive stress on the ceramic sintered body substrate 110, and as a result, due to the frictional force acting between the ceramic sintered body substrate 110 and the solidified sprayed particles, the ceramic sintered body substrate 110 and the insulating ceramic sprayed film 140 are in a state of being adhered. The absence of a chemical bond between the elements constituting the ceramic sintered body substrate 110 and the insulating ceramic sprayed film 140 can be confirmed by the fact that no reaction layer is formed between the ceramic sintered body substrate 110 and the insulating ceramic sprayed film 140.
[0045] [Second Embodiment] (Configuration of the Sprayed Film Coating Member) Next, the sprayed film coating member according to the second embodiment of the present invention will be described with reference to FIGS. 5 and 6. FIGS. 5 and 6 are schematic cross-sectional views showing an example of the sprayed film coating member according to the second embodiment of the present invention. The sprayed film coating member 100 according to the present embodiment has the same basic configuration as the sprayed film coating member 100 according to the first embodiment, and includes a ceramic sintered body substrate 110, a metal base 120, and an insulating ceramic sprayed film 140.
[0046] The insulating ceramic sprayed film 140 of the thermal spraying film covering member 100 according to this embodiment has a two-layer structure with different textures. As a result, the thickness of the insulating ceramic sprayed film 140 can be increased, and the withstand voltage characteristics of the insulating ceramic sprayed film 140 can be improved. As a result, creeping discharge can be further suppressed.
[0047] That the insulating ceramic sprayed film 140 has a two-layer structure with different textures means that the insulating ceramic sprayed film 140 is composed of a first insulating ceramic sprayed film 141 formed on a specific surface 122 of the metal base 120, a surface 152 of the bonding interface between the ceramic sintered body base material 110 and the metal base 120, and a surface 112 of the ceramic sintered body base material near the surface 152 of the bonding interface, and a second insulating ceramic sprayed film 142 formed on the surface of the first insulating ceramic sprayed film 141.
[0048] The first insulating ceramic sprayed film 141 is continuously formed on a specific surface 122 of the metal base 120, a surface 152 of the bonding interface between the ceramic sintered body base material 110 and the metal base 120, and a surface 112 of the ceramic sintered body base material near the surface 152 of the bonding interface. Further, the second insulating ceramic sprayed film 142 is preferably continuously formed on the surface of the first insulating ceramic sprayed film 141. The second insulating ceramic sprayed film 142 does not have to be formed on the entire surface of the surface of the first insulating ceramic sprayed film 141.
[0049] That the insulating ceramic sprayed film 140 has a two-layer structure with different textures can be confirmed, for example, by the difference in porosity. In this case, the porosity of the first insulating ceramic sprayed film 141 is preferably 0.5% or more and less than 4%, and more preferably 0.5% or more and 3% or less. Further, the porosity of the second insulating ceramic sprayed film 142 is preferably 4% or more and 7% or less.
[0050] The first and second insulating ceramic sprayed films 141 and 142 can be selected from various materials. For example, specifically, it is the same as the material of the insulating ceramic sprayed film 140 of the first embodiment. The first insulating ceramic sprayed film 141 may be composed of two or more combinations. Composed of two or more combinations means that the first insulating ceramic sprayed film 141 is formed by a mixture of particles made of different raw materials. The same applies to the second insulating ceramic sprayed film 142. The first insulating ceramic sprayed film 141 and the second insulating ceramic sprayed film 142 may be made of the same material or different materials.
[0051] The thickness in the direction perpendicular to the specific surface 122 of the metal base 120 of the insulating ceramic sprayed film 140 is preferably 50 μm or more. Thereby, sufficient withstand voltage characteristics can be obtained and creeping discharge can be suppressed. In this embodiment, the thickness in the direction perpendicular to the specific surface 122 of the metal base 120 of the insulating ceramic sprayed film 140 is the thickness of the insulating ceramic sprayed film 140 at the position where both the first insulating ceramic sprayed film 141 and the second insulating ceramic sprayed film 142 are formed on the specific surface 122 of the metal base 120. There is no particular need to define the upper limit of the thickness in the direction perpendicular to the specific surface 122 of the metal base 120 of the insulating ceramic sprayed film 140, but for example, it can be 520 μm or less.
[0052] The thickness in the direction perpendicular to the specific surface 122 of the metal base 120 of the first insulating ceramic sprayed film 141 is preferably 10 μm or more and 20 μm or less. Thereby, the risk of peeling of the first insulating ceramic sprayed film 141 can be reduced. Also, the thickness in the direction perpendicular to the specific surface 122 of the metal base 120 of the second insulating ceramic sprayed film 142 is preferably 40 μm or more and 500 μm or less. Thereby, the thickness of the insulating ceramic sprayed film 140 can be increased, and the withstand voltage characteristics of the insulating ceramic sprayed film 140 can be improved. As a result, creeping discharge can be more effectively suppressed.
[0053] The space volume Vvv (μm 3 / μm 2 ) of the surface to be sprayed of the ceramic sintered body substrate 110 (the surface 112 of the ceramic sintered body substrate near the surface 152 of the bonding interface), and the average particle size D50 (μm) of the ceramic raw material for forming the insulating ceramic sprayed film 140 (the first insulating ceramic sprayed film 141) on the ceramic sintered body substrate 110 side satisfy 0.001 ≦ (Vvv / (D50) 3 ) ≦ 0.40 is preferable.
[0054] Thereby, the ceramic sintered body substrate 110 and the first insulating ceramic sprayed film 141 are likely to adhere to each other, and the durability of the sprayed film covering member 100 is increased. Also, AlN or Al 2 O 3 which is difficult to adhere to the insulating ceramic sprayed film 140 can be used as the material of the ceramic sintered body substrate 110, and the applications of the sprayed film covering member 100 are widened.
[0055] The sprayed film covering member 100 of the present invention can be a member in which creeping discharge is suppressed and the insulation performance is improved.
[0056] [Manufacturing method of sprayed film covering member] (Preparation of ceramic sintered body substrate) Figs. 7(a) to (c) are schematic cross-sectional views showing one step of the manufacturing process of the sprayed film covering member according to the first embodiment of the present invention. First, a ceramic sintered body substrate 110 is prepared. The ceramic sintered body substrate 110 can be formed of various materials.
[0057] The ceramic sintered body substrate 110 may be produced by any method. The manufacturing conditions are appropriately selected according to the type of raw material of the substrate. For example, the atmospheric pressure sintering method, the hot pressing method, or HIP can be used. For example, when using the hot pressing method, a molded body can be produced by molding a mixed powder of raw material powder and sintering aid powder, and the ceramic sintered body substrate 110 can be produced by firing this. For example, when using AlN as a raw material, the firing temperature is adjusted to be included in the temperature range of 1650 to 1950 °C, more preferably in the temperature range of 1750 to 1900 °C. The firing time (holding time at the firing temperature) is adjusted to be included in the time range of 2 to 10 hours. The pressing pressure during firing is adjusted to be included in the pressure range of 1 to 15 MPa. Note that these firing temperatures and firing times are changed depending on the type and addition amount of the raw material powder and sintering aid powder, etc.
[0058] (First adjustment step) Next, the space volume Vvv (μm 3 / μm 2 ) of the sprayed surface (the surface 112 of the ceramic sintered body substrate near the surface 152 of the bonding interface) of the prepared ceramic sintered body substrate 110 is adjusted to a predetermined range. The sprayed surface of the prepared ceramic sintered body substrate 110 is adjusted to a predetermined range by performing processing such as polishing or grinding. In this specification, the space volume Vvv refers to the void volume of the valley portion at a load area ratio of 80%. The space volume Vvv (μm 3 / μm 2 ) can be measured in accordance with ISO 25178 using a coherence correlation interferometer or the like.
[0059] The surface to be sprayed may be processed by blasting, but depending on the abrasive used and the spraying intensity, minute cracks may occur in non-metal substrates such as the ceramic sintered body substrate 110. Due to such cracks, there is a risk of a decrease in the strength of the substrate material or substrate breakage caused by the cracks. Therefore, when performing blasting, sufficient attention must be paid. That is, when performing blasting, it should be carried out so that cracks do not occur according to the material of the substrate etc. Since the method of the present invention does not require roughening the surface to be sprayed of the ceramic sintered body substrate 110, it is not necessary to perform blasting at a spraying intensity that causes cracks. Therefore, it is also possible to use blasting after adjusting the strength.
[0060] However, in the case of polishing or grinding, since there is little risk of the problem cracks occurring, when processing the surface to be sprayed of the ceramic sintered body substrate 110, it is preferable that it is polishing or grinding. Also, when the spatial volume Vvv of the surface to be sprayed of the ceramic sintered body substrate 110 is within a predetermined range in the state of the fired surface after sintering, processing may not be performed.
[0061] The adjustment of the surface to be sprayed is such that 0.001 ≦ (Vvv / (D50) 3 ) ≦ 0.40 with respect to the spatial volume Vvv and the average particle diameter D50 according to the average particle diameter D50 of the ceramic raw material powder contained in the slurry used in the coating process described later. This adjustment may be made by measuring the spatial volume Vvv after processing the surface to be sprayed based on the average particle diameter D50 of the ceramic raw material powder used, and if it is not within the above range, further processing the surface to be sprayed, or by measuring the spatial volume Vvv after processing the surface to be sprayed and adjusting by changing the ceramic raw material powder used based on the measurement result of the spatial volume Vvv. Note that the spatial volume Vvv (μm 3 / μm 2 ) is preferably 0.01 or more and 0.30 or less.
[0062] (Preparation of Metal Base) Separate from the preparation of the ceramic sintered body substrate 110, a metal base 120 is prepared. The metal base 120 can be made of various materials.
[0063] (Second adjustment step) Next, the surface roughness Sa (μm) of the sprayed surface (a specific surface 122 of the metal base 120) of the prepared metal base 120 is adjusted to a predetermined range. The sprayed surface of the prepared metal base 120 is adjusted to the predetermined range by, for example, blasting. The surface roughness Sa of the sprayed surface of the metal base 120 is preferably 1.5 μm or more and 5.0 μm or less. Since it is better to set the numerical range up to the vicinity of the bonding interface 150 for the first adjustment step and the second adjustment step, it is preferably performed before the bonding step. On the other hand, in the case of specific circumstances such as directly adopting bonding in the bonding step and performing bonding with the metal base 120 simultaneously during the sintering of the ceramic sintered body substrate 110, the first adjustment step and the second adjustment step may be performed after the bonding step.
[0064] (Bonding step) Next, the prepared ceramic sintered body substrate 110 and the metal base 120 are bonded to form a bonded body 130. The bonding between the ceramic sintered body substrate 110 and the metal base 120 can be selected from various bonding methods.
[0065] (Coating step) Next, an insulating ceramic raw material powder having an average particle diameter D50 in the range of 0.5 μm or more and 10 μm or less and water are prepared and mixed to adjust a slurry. The average particle diameter D50 of the insulating ceramic raw material powder is preferably 0.5 μm or more and 10 μm or less. When D50 is smaller than 0.5 μm, the viscosity of the slurry becomes high, making spraying difficult and deteriorating the film quality. Also, when it is larger than 10 μm, the slurry cannot be stably transported, deteriorating the film quality. The average particle diameter D50 can be measured using dry measurement or wet measurement of a laser diffraction / scattering particle size distribution measuring device. The particle size distribution of the insulating ceramic raw material powder is preferably sharp.
[0066] Insulating ceramic raw material powder can use various materials. The insulating ceramic raw material powder is, for example, Al 2 O 3 (alumina), Y 2 O 3 (yttria), YAG (Y 3 Al 5 O 12 : yttrium aluminum garnet), TiO 2 (titania), Cr 2 O 3 (chromia), silicon nitride (Si 3 N 4 ), aluminum nitride (AlN), or powders of insulating ceramics such as these or any mixed powders thereof can be used. Since the ceramic sintered body substrate 110 is formed of a ceramic sintered body, depending on its material, the adhesion of the insulating ceramic sprayed film 140 may become a problem. The manufacturing method of the present invention can form an insulating ceramic sprayed film 140 with high adhesion using these materials while reducing the risk of strength reduction and breakage of the ceramic sintered body substrate 110 even for the ceramic sintered body substrate 110.
[0067] The concentration of the slurry is preferably 10 wt% or more and 40 wt% or less, and more preferably 20 wt% or more and 40 wt% or less. When the concentration of the slurry is less than 10 wt%, it takes time for construction and productivity is reduced, so it is not industrial. Also, when it is more than 40 wt%, the viscosity becomes high and the slurry cannot be stably transported.
[0068] Then, the adjusted slurry is plasma sprayed and coated on the sprayed surface of the joined body 130 (the specific surface 122 of the metal base, the surface 152 of the joining interface between the ceramic sintered body substrate 110 and the metal base 120, and the surface 112 of the ceramic sintered body substrate near the surface 152 of the joining interface). The gas used for spraying is preferably a non-oxidizing gas. As the non-oxidizing gas, for example, Ar gas, H 2 gas or N 2A mixed gas of gas or any combination thereof can be used. The above slurry is supplied to a nozzle via a tube pump and is plasma sprayed using the gas.
[0069] Before the step of plasma spraying, a step of plasma irradiating the surface to be sprayed of the joined body 130 with only the gas without introducing the slurry may be provided. By providing such a step, the surface to be sprayed of the joined body 130 is preheated, and when plasma spraying is performed, the molten ceramic raw material powder easily penetrates into the voids.
[0070] As a result, an insulating ceramic sprayed film 140 derived from the slurry is formed on a specific surface 122 of the metal base, a surface 152 of the joining interface between the ceramic sintered body base material 110 and the metal base 120, and a surface 112 of the ceramic sintered body base material in the vicinity of the surface 152 of the joining interface. Although it is often difficult to continuously form the insulating ceramic sprayed film 140 via the surface 152 of the joining interface on both the ceramic sintered body base material 110 and the metal base 120 having different properties, the manufacturing method of the present invention can continuously form the insulating ceramic sprayed film 140 even for the joined body 130 made of materials having different properties.
[0071] (Second coating step) The manufacturing method of the sprayed film coating member 100 according to the second embodiment uses the above coating step as the first coating step, and then performs a second coating step. In the second coating step, a second insulating ceramic raw material powder is sprayed on the surface of the first insulating ceramic sprayed film 141 to form a second insulating ceramic sprayed film 142. The second coating step is performed by a spraying method different from that of the first coating step. The second coating step can use known spraying methods such as atmospheric plasma spraying (APS), flame spraying, and high velocity oxy-fuel (HVOF).
[0072] The second insulating ceramic raw material powder used in the second coating process can be made of various materials, similar to the above-mentioned insulating ceramic raw material powder (the first insulating ceramic raw material powder). The second insulating ceramic raw material powder preferably consists of granules. The average particle diameter D50 of the second insulating ceramic raw material powder is preferably 10 μm or more and 70 μm or less.
[0073] In the manufacturing method of the present invention, the size of the space volume Vvv of the sprayed surface of the ceramic sintered body substrate 110 is compatible with the average particle diameter D50 of the insulating ceramic raw material powder. Therefore, even when the ceramic sintered body substrate 110 is a brittle material and is an AlN sintered body, an SiC sintered body, or an Al sintered body made of a material with poor adhesion to other ceramic materials, the molten particles obtained by melting the particles of the insulating ceramic raw material powder penetrate into the voids of several micrometers or less remaining on the surface of the substrate in an appropriate amount, and pancakes (splats) are formed with these as nuclei, enabling adhesion to the ceramic sintered body substrate 110. Furthermore, sufficient strength adhesion can also be achieved on the surface of the bonding interface 150 between the ceramic sintered body substrate 110 and the metal base 120 and on the surface of the metal base 120. As a result, the insulating ceramic sprayed film 140 can be continuously formed on the specific surface 122 of the metal base 120, the surface 152 of the bonding interface between the ceramic sintered body substrate 110 and the metal base 120, and the surface 112 of the ceramic sintered body substrate near the surface 152 of the bonding interface. 2 O 3 By such a manufacturing method, a sprayed film coating member 100 with improved insulation performance and suppressed surface discharge can be manufactured.
[0074]
[0075] [Examples and Comparative Examples] (Example 1) (Ceramic Sintered Body Substrate Preparation Step, First Adjustment Step) Y was added as a sintering aid to AlN raw material powder with a purity of 99% and an average particle diameter of 0.5 μm, 2 O 3 and an organic binder, and by the CIP (Cold Isostatic Pressing) forming method, at 1 ton / cm 2 Hydrostatic pressure forming was performed to produce an AlN compact. Next, the AlN compact was sintered at 1950 °C for 4 hours under atmospheric pressure in an N 2 atmosphere to produce an AlN sintered body. Next, the AlN sintered body was processed into a substantially rectangular plate shape (substantially square plate shape) of □20 mm × thickness 5 mm to produce an AlN sintered body substrate (ceramic sintered body substrate).
[0076] At this time, by polishing the side surface (sprayed surface) of the AlN sintered body substrate, its surface roughness Sa was adjusted to 0.90 μm, and its spatial volume Vvv (μm 3 / μm 2 ) was adjusted to 0.17. By setting the average particle diameter D50 of the raw material powder used in the coating process described later to 3 μm, the value of (Vvv / (D50) 3 ) was adjusted to 0.0063. The spatial volume Vvv was measured using a coherence correlation interferometer (manufactured by Taylor Hobson).
[0077] (Metal base preparation process, second adjustment process) Separately from this, as a metal base, a substantially rectangular plate shape (substantially square plate shape) of Mo (purity 99.9%) with □20 mm × thickness 5 mm was prepared. At this time, by processing one main surface that becomes the bonding surface with the AlN sintered body substrate of the metal base, its surface roughness Sa was adjusted to 0.4 μm. Also, by blasting the side surface (sprayed surface) of the metal base, its surface roughness Sa was adjusted to 3.0 μm.
[0078] (Bonding process) One main surface of the metal base was overlapped with the AlN sintered body substrate, and it was held at 1800 °C under a pressure of 4 MPa perpendicular to one main surface to bond the AlN sintered body substrate and the metal base to produce a bonded body. The thickness of the bonding layer at the bonding interface was less than 5 μm.
[0079] (Plasma irradiation process) Next, a non-oxidizing gas plasma was irradiated or injected onto the surface to be sprayed of the joined body using a high-speed plasma spraying machine to preheat the surface to be sprayed. The surface to be sprayed of the joined body is the surface to be sprayed of the AlN sintered body substrate, the surface of the joining interface between the AlN sintered body substrate and the metal base, and the surface to be sprayed of the metal base. As the non-oxidizing gas, a mixed gas of Ar gas, N 2 gas and H 2 gas was used. The supply amount of Ar gas to the nozzle constituting the spraying machine was controlled to 100 l / min, and the supply amount of N 2 gas was controlled to 70 l / min, and the supply amount of H 2 gas was controlled to 70 l / min.
[0080] By controlling the applied current to the nozzle constituting the high-speed plasma spraying machine to 250 A, the supply power to the nozzle was adjusted to 65 kW. The distance between the tip of the nozzle and the surface to be sprayed of the joined body was adjusted to 75 mm. The scanning speed or displacement speed of the nozzle with respect to the joined body was adjusted to 850 mm / s. As a result, a plasma of a mixed gas of Ar gas, N 2 gas and H 2 gas was generated, and the plasma was irradiated or injected from the tip of the nozzle onto the surface to be sprayed of the joined body. The preheating of the surface to be sprayed by the irradiation or injection of the plasma was performed for 3 minutes.
[0081] (Coating process) Then, using the high-speed plasma spraying machine as it is, Al 2 O 3 slurry was plasma-sprayed onto the surface to be sprayed of the joined body using a non-oxidizing gas. The slurry was prepared by mixing 300 g of raw material powder of Al 2 O 3 with a purity of 99.9% or more and an average particle size D50 of 3 μm and 700 g of water to adjust the Al 2 O 3 slurry. As the non-oxidizing gas, a mixed gas of Ar gas, N 2 gas and H 2 gas was used. The supply amount of Ar gas to the nozzle constituting the spraying machine was controlled to 100 l / min, and N 2The supply rate of the gas was controlled to 70 l / min, and H 2 The supply rate of the gas was controlled to 60 l / min. As a result, the spraying speed was controlled to 600 - 700 mm / s.
[0082] By controlling the applied current to the nozzle constituting the high - speed plasma spraying machine to 250 A, the power supplied to the nozzle was adjusted to 65 kW. The distance between the tip of the nozzle and the sprayed surface of the joined body was adjusted to 75 mm. The scanning speed or displacement speed of the nozzle with respect to the joined body was adjusted to 850 mm / s. As a result, plasma of a mixed gas of Ar gas, N 2 gas and H 2 gas was generated, and the raw material powder melted by the plasma was sprayed from the tip of the nozzle onto the sprayed surface of the joined body. The introduction amount of the slurry was controlled to 30 g / min. Plasma spraying was performed so that the thickness of the insulating ceramic sprayed film would be 100 μm. Thus, two samples of the sprayed film - coated member of Example 1, in which the entire side surface of the AlN sintered body substrate, the surface of the joining interface between the AlN sintered body substrate and the metal base, and the entire side surface of the metal base were covered with an insulating ceramic sprayed film composed of Al 2 O 3 were formed.
[0083] (Example 2) Example 2 is an example in which the type of raw material of the insulating ceramic sprayed film is different from that of Example 1. In the coating process, the raw material powder constituting the slurry was changed from Al 2 O 3 raw material powder to Y 2 O 3 powder. Otherwise, two samples of the sprayed film - coated member of Example 2 were formed under the same conditions as in Example 1.
[0084] (Example 3) Example 3 is an example in which the type of metal base and the joining method are different from those of Example 1. In the metal base preparation process, the metal base was changed from Mo to Al (purity 99.9%). In the joining process, the joining between the AlN sintered body base material and the metal base was changed from direct joining to joining with a silicone adhesive. The thickness of the joining layer at the joining interface was 50 μm. Two samples of the sprayed film coated member of Example 3 were formed under the same conditions as Example 1 except for the above.
[0085] Example 4 Example 4 is an example in which the structure of the insulating ceramic sprayed film is different from that of Example 1. In the coating step, an insulating ceramic sprayed film (first insulating ceramic sprayed film) was formed to a thickness of 10 μm, and then a second coating step was carried out.
[0086] (Second coating process) The second coating process was carried out by atmospheric plasma spraying. The high-velocity plasma spraying machine was used to spray Al. 2 O 3 The granules were air plasma sprayed onto the surface of the first insulating ceramic sprayed film of the joint body using an oxidizing gas. 2 O 3 The granules are made of Al with a purity of 99.9% or more and an average particle size D50 of 35 μm. 2 O 3 The raw material powder was used. Ar gas and O were used as oxidizing gases. 2 The amount of Ar gas supplied to the nozzle of the thermal spraying machine was controlled at 70 l / min, and O 2 The gas supply was controlled at 10 l / min, which controlled the spraying speed at 500 to 600 mm / s.
[0087] The current applied to the nozzle constituting the high-speed plasma spraying machine was controlled to 250 A, and the power supplied to the nozzle was adjusted to 65 kW. The distance between the tip of the nozzle and the surface of the first insulating ceramic sprayed film of the joint was adjusted to 75 mm. The scanning speed or displacement speed of the nozzle relative to the joint was adjusted to 850 mm / s. This allowed the Ar gas, O 2 Gas and H2 A plasma of a gas mixture was generated, and the raw material powder melted by the plasma was sprayed from the tip of the nozzle onto the surface of the first insulating ceramic sprayed film of the joined body. The introduction amount of the granules was controlled to 30 g / min. Atmospheric plasma spraying was performed so that the thickness of the second insulating ceramic sprayed film became 250 μm. Other than these, two samples of the sprayed film covering member of Example 4 were formed under the same conditions as in Example 1.
[0088] (Example 5) Example 5 is an example in which the type of the metal base, the joining method, and the thickness of the insulating ceramic sprayed film are different from those in Example 4. In the metal base preparation step, the metal base was changed from being made of Mo to being made of Al (purity 99.9%). Also, in the joining step, the joining of the AlN sintered body base material and the metal base was changed from direct joining to joining with an Al foil. The thickness of the joining layer at the joining interface was 200 μm. Also, the thickness of the first insulating ceramic sprayed film was 20 μm, and the thickness of the second insulating ceramic sprayed film was 500 μm. Other than these, two samples of the sprayed film covering member of Example 5 were formed under the same conditions as in Example 4.
[0089] (Example 6) Example 6 is an example in which the joining method is different from that in Example 1. In the joining step, the joining of the AlN sintered body base material and the metal base was changed from direct joining to joining with an Al foil. The thickness of the joining layer at the joining interface was 200 μm. Other than these, two samples of the sprayed film covering member of Example 6 were formed under the same conditions as in Example 1.
[0090] (Example 7) Example 7 is an example in which the space volume Vvv and the average particle diameter D50 are different from those in Example 6. In the first adjustment step, the space volume Vvv was adjusted to 0.05 by polishing the sprayed surface of the AlN sintered body base material. Also, by setting the average particle diameter D50 of the raw material powder contained in the slurry to 6 μm, the value of (Vvv / (D50) 3 ) was adjusted to 0.0002. Other than these, two samples of the sprayed film covering member of Example 7 were formed under the same conditions as in Example 6.
[0091] (Example 8) Example 8 is an example where the spatial volume Vvv and the average particle diameter D50 are different from those in Example 6. In the first adjustment step, the surface to be sprayed of the AlN sintered body substrate was polished to adjust the spatial volume Vvv to 0.99. Also, by setting the average particle diameter D50 of the raw material powder contained in the slurry to 10 μm, the value of (Vvv / (D50) 3 ) was adjusted to 0.0010. Otherwise, two samples of the sprayed film coating member of Example 8 were formed under the same conditions as in Example 6.
[0092] (Example 9) Example 9 is an example where the spatial volume Vvv and the average particle diameter D50 are different from those in Example 6. In the first adjustment step, the surface to be sprayed of the AlN sintered body substrate was polished to adjust the spatial volume Vvv to 0.05. Also, the average particle diameter D50 of the raw material powder contained in the slurry was adjusted to 0.5 μm. As a result, the value of (Vvv / (D50) 3 ) was adjusted to 0.4000. Otherwise, two samples of the sprayed film coating member of Example 9 were formed under the same conditions as in Example 6.
[0093] (Example 10) Example 10 is an example where the spatial volume Vvv and the average particle diameter D50 are different from those in Example 6. In the first adjustment step, the surface to be sprayed of the AlN sintered body substrate was polished to adjust the spatial volume Vvv to 0.51. Also, the average particle diameter D50 of the raw material powder contained in the slurry was adjusted to 1.0 μm. As a result, the value of (Vvv / (D50) 3 ) was adjusted to 0.5100. Otherwise, two samples of the sprayed film coating member of Example 10 were formed under the same conditions as in Example 6.
[0094] (Example 11) Example 11 is an example in which the spatial volume Vvv, the surface roughness Sa of the metal base, and the thickness of the insulating ceramic sprayed film are different from those of Example 1. In the first adjustment step, the sprayed surface of the AlN sintered body substrate was polished to adjust the spatial volume Vvv to 0.13. As a result, the value of (Vvv / (D50) 3 ) was adjusted to 0.1111. Also, in the second adjustment step, the sprayed surface of the metal base was processed to adjust the surface roughness Sa to 2.0 μm. Otherwise, two samples of the sprayed film covering member of Example 11 were formed under the same conditions as in Example 1.
[0095] (Example 12) Example 11 is an example in which the spatial volume Vvv, the surface roughness Sa of the metal base, and the thickness of the insulating ceramic sprayed film are different from those of Example 1. In the first adjustment step, the sprayed surface of the AlN sintered body substrate was polished to adjust the spatial volume Vvv to 0.25. As a result, the value of (Vvv / (D50) 3 ) was adjusted to 0.1111. Also, in the second adjustment step, the sprayed surface of the metal base was processed to adjust the surface roughness Sa to 5.0 μm. Otherwise, two samples of the sprayed film covering member of Example 11 were formed under the same conditions as in Example 1.
[0096] (Comparative Example 1) Comparative Example 1 is a comparative example in which an insulating ceramic sprayed film was not formed. In the first adjustment step and the second adjustment step, the sprayed surface was not adjusted either. Otherwise, two samples of the joined body of Comparative Example 1 were formed under the same conditions as in Example 1.
[0097] (Comparative Example 2) Comparative Example 2 is a comparative example in which an insulating ceramic sprayed film was formed only on the entire side surface of the metal base. Otherwise, two samples of the joined body of Comparative Example 2 were formed under the same conditions as in Example 1.
[0098] (Various Measurements) Measurements were made on samples of the thermal spray film-coated members of the examples and samples of the bonded bodies of the comparative examples. Figure 8 is a table showing the manufacturing conditions and the results of the withstand voltage tests for the samples of the thermal spray film-coated members of the examples and the samples of the bonded bodies of the comparative examples.
[0099] (Film thickness measurement) The thickness of the insulating ceramic thermal spray film on the sprayed surface of the metal base was measured with an eddy current type film thickness gauge.
[0100] (Withstand voltage test) For two samples of the thermal spray film-coated members of the examples and two samples of the bonded bodies of the comparative examples, the withstand voltage in vacuum (1 Pa) and the withstand voltage in air were measured for one of each. For each sample, the metal base was grounded, and a Φ1 mm needle-shaped probe connected to a high-voltage power supply was brought into contact with the insulating ceramic thermal spray film on the AlN sintered body substrate in the examples and the AlN sintered body substrate in the comparative examples, and the voltage was increased. Then, using an evaluation machine (high-voltage power supply) (HIGH VOLTAGE POWER SUPPLY manufactured by Matsueda Precision, model number: HARb-20R3), the respective withstand voltages in vacuum and in air were measured under the conditions of direct current, Rate: 0.1 V·s -1 The respective withstand voltages in vacuum and in air were measured.
[0101] The pass / fail criteria for the withstand voltage were determined as follows. For the results of the withstand voltage test in vacuum, if it was 40 V·μm -1 or more, and for the results of the withstand voltage test in air, if it was 30 V·μm -1 or more, it was rated as excellent (◎). Among those that did not meet the excellent criteria, for the results of the withstand voltage test in vacuum, if it was 25 V·μm -1 or more, and for the results of the withstand voltage test in air, if it was 20 V·μm -1 it was rated as good (○). Among those that did not meet the excellent and good criteria, for the results of the withstand voltage test in vacuum, if it was 20 V·μm -1 or more, and for the results of the withstand voltage test in air, if it was 15 V·μm -1 it was rated as acceptable (△), and these were considered to have passed. Also, those that did not meet any of the excellent, good, or acceptable criteria were rated as failed (×).
[0102] The thermal spray film-coated members of Examples 1 to 12 all had excellent or good results in the withstand voltage test. In contrast, the joined body of Comparative Example 1 failed the withstand voltage test, and the joined body of Comparative Example 2 had a pass result in the withstand voltage test, both of which were worse than the thermal spray film-coated members of the examples. Thus, it was confirmed that by continuously forming an insulating ceramic thermal spray film on a specific surface of the metal base of the joined body, the surface of the joining interface between the ceramic sintered body base material and the metal base, and the surface of the ceramic sintered body base material in the vicinity of the surface of the joining interface, the insulation of the joined body was improved.
[0103] Among Examples 1 to 12, for the space volume Vvv (μm 3 / μm 2 ) of the surface to be thermally sprayed of the ceramic sintered body base material and the average particle diameter D50 (μm) of the ceramic raw material for forming the insulating ceramic thermal spray film or the first insulating ceramic thermal spray film, Examples 1 to 5, 8, 9, 11, and 12 in which the value of (Vvv / (D50) 3 ) was adjusted to be 0.001 or more and 0.40 or less had excellent results in the withstand voltage test. This is presumably because the adhesion of the insulating ceramic thermal spray film to the ceramic sintered body base material was good. Thus, for the space volume Vvv (μm 3 / μm 2 ) of the surface to be thermally sprayed of the ceramic sintered body base material and the average particle diameter D50 (μm) of the ceramic raw material for forming the insulating ceramic thermal spray film or the first insulating ceramic thermal spray film, it was confirmed that the value of (Vvv / (D50) 3 ) was preferably adjusted to be 0.001 or more and 0.40 or less.
[0104] Comparing Example 5 and Example 6, for the thickness D of the insulating ceramic thermal spray film and the thickness G of the joining layer at the joining interface, Example 5 in which G < D was satisfied had better results in the withstand voltage test. Thus, it was confirmed that it was preferable to satisfy G < D.
[0105] The present invention is not limited to the above-described embodiments, and it goes without saying that the present invention extends to various modifications and equivalents included in the spirit and scope of the present invention. In addition, the structure, shape, number, position, size, etc. of the components shown in each drawing are for convenience of explanation and can be changed as appropriate.
Explanation of Signs
[0106] 100 Thermal spraying film coating member 110 Ceramic sintered body base material 112 Surface of the ceramic sintered body base material 120 Metal base 122 Specific surface 130 Bonded body 140 Insulating ceramic thermal spraying film 141 First insulating ceramic thermal spraying film 142 Second insulating ceramic thermal spraying film 150 Bonding interface 152 Surface of the bonding interface
Claims
1. A thermal sprayed film-coated member, comprising: a ceramic sintered body substrate; a metal base joined to the ceramic sintered body substrate; an insulating ceramic thermal sprayed film continuously formed on a specific surface of the metal base, a surface of a bonding interface between the ceramic sintered body substrate and the metal base, and a surface of the ceramic sintered body substrate in the vicinity of the surface of the bonding interface.
2. The thermal sprayed film-coated member according to claim 1, wherein the insulating ceramic thermal sprayed film has a porosity of 0.5% or more and 7% or less.
3. The thermal sprayed film-coated member according to claim 1, wherein the insulating ceramic thermal sprayed film has a two-layer structure with different microstructures.
4. The thermal sprayed film-coated member according to any one of claims 1 to 3, wherein a thickness of the insulating ceramic thermal sprayed film in a direction perpendicular to a specific surface of the metal base is 50 μm or more.
5. The space volume Vvv (μm 3 / μm 2 ) of the sprayed surface of the ceramic sintered body substrate and the average particle diameter D50 (μm) of the ceramic raw material for forming the insulating ceramic sprayed film satisfy 0.001 ≤ (Vvv / (D50)) 3 ≤ 0.40 The thermal sprayed film-coated member according to claim 1, characterized by satisfying
6. The space volume Vvv (μm 3 / μm 2 ) of the sprayed surface of the ceramic sintered body substrate and the average particle diameter D50 (μm) of the ceramic raw material for forming the insulating ceramic sprayed film on the ceramic sintered body substrate side, 0.001 ≤ (Vvv / (D50)) 3 ≤ 0.40 The thermal sprayed film-coated member according to claim 3, characterized by satisfying
7. A method for manufacturing a thermal sprayed film-coated member, comprising: The first adjustment step of adjusting the spatial volume Vvv (μm 3 / μm 2 ) of the sprayed surface of the ceramic sintered body substrate to a predetermined range, a second adjusting step of adjusting a surface roughness Sa (μm) of a surface to be thermally sprayed of a metal base to a predetermined range; a bonding step of bonding the ceramic sintered body substrate and the metal base; a coating step of forming an insulating ceramic thermal sprayed film by plasma spraying a slurry composed of water and an insulating ceramic raw material powder having an average particle diameter D50 in a range of 0.5 μm or more and 10 μm or less on a surface to be thermally sprayed of the ceramic sintered body substrate, a surface of a bonding interface between the ceramic sintered body substrate and the metal base, and a surface to be thermally sprayed of the metal base, wherein the first adjusting step adjusts the space volume Vvv and the average particle diameter D50 to 0.001 ≤ (Vvv / (D50)) 3 ≤ 0.40 be in a range of
8. A method for manufacturing a thermal sprayed film-coated member, comprising: The spatial volume Vvv (μm 3 / μm 2 ) of the sprayed surface of the ceramic sintered body substrate is adjusted to a predetermined range in a first adjustment step, and a second adjusting step of adjusting a surface roughness Sa (μm) of a surface to be thermally sprayed of a metal base to a predetermined range; a bonding step of bonding the ceramic sintered body substrate and the metal base; A first coating step of forming a first insulating ceramic sprayed film by plasma spraying a first slurry composed of water and a first insulating ceramic raw material powder having an average particle diameter D50 in the range of 0.5 μm or more and 10 μm or less onto the sprayed surface of the ceramic sintered body base material, the surface of the bonding interface between the ceramic sintered body base material and the metal base, and the sprayed surface of the metal base; A second coating step of forming a second insulating ceramic sprayed film by spraying a second insulating ceramic raw material powder onto the surface of the first insulating ceramic sprayed film; The first adjustment step is for the space volume Vvv and the average particle diameter D50; 0.001 ≤ (Vvv / (D50)) 3 ≤ 0.40 A method for manufacturing a sprayed film coating member, characterized in that it is adjusted so as to be in the range of.
Citation Information
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Thermal spraying member
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