Conjugate

Abstract

A joint of a ceramic plate and an MMC plate having high joint strength is provided, the joint comprising: a ceramic plate; an MMC plate made of a metal matrix composite (MMC) provided opposite one side of the ceramic plate; and a joint layer provided between the ceramic plate and the MMC plate for joining the ceramic plate and the MMC plate, the joint layer containing Al as a main component and Si and Mg as minor components, and a joint interface between the ceramic plate and the joint layer containing an Mg-containing layer.

Description

[Technical field]

[0001] The present disclosure relates to conjugates. [Background technology]

[0002] In semiconductor device manufacturing, circuit formation is generally performed by plasma etching. Plasma etching is performed by introducing an inert gas into a vacuum chamber in a plasma etching apparatus to generate plasma. An electrostatic chuck assembly is provided in the plasma etching apparatus, which functions as a susceptor on which a wafer to be etched is placed. A typical electrostatic chuck assembly includes an electrode-embedded ceramic plate that functions as an electrostatic chuck, and a cooling plate that supports the bottom surface of the electrode-embedded ceramic plate. The wafer is electrostatically attracted to the electrode-embedded ceramic plate, and plasma etching is performed while the wafer is fixed to the electrostatic chuck assembly. Meanwhile, the cooling plate is provided on the bottom surface of the electrode-embedded ceramic plate, and is configured to remove heat generated in the wafer by plasma etching. The electrode-embedded ceramic plate generally has a configuration in which internal electrodes such as an electrostatic chuck (ESC) electrode, an RF electrode, and a heater electrode are embedded inside a ceramic base made of aluminum oxide, aluminum nitride, or the like, which has excellent heat resistance and corrosion resistance.

[0003] As an example of an electrostatic chuck assembly, Patent Document 1 (JP 2009-141204 A) discloses a substrate holder in which a first base made of a first ceramic sintered body and a second base made of a second ceramic sintered body are bonded via a bonding film of a metal containing Al. This document discloses that the first base and the second base are bonded via the bonding film by sandwiching a bonding film of a metal containing Al between the first base and the second base and heating the metal and thermocompressing the metal at a pressure of 4 to 20 MPa, and it is stated that the metal containing Al is preferably an Al alloy containing 0.5 to 5 wt % Mg.

[0004] Meanwhile, metal matrix composites (MMCs) have been attracting attention in recent years. Metal matrix composites are materials in which a ceramic reinforcing material such as SiC or TiC is combined with a metal matrix made of metals such as Al or metal Si, and are known to have advantages such as light weight, high rigidity, high thermal conductivity, and low thermal expansion. A method for joining a metal matrix composite (MMC) to a ceramic material has been proposed, and Patent Document 2 (Japanese Patent No. 4373538) discloses a joined body in which an MMC containing an aluminum alloy as a matrix and a ceramic material are joined via a brazing material made of an Al alloy containing Mg. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] JP 2009-141204 A [Patent Document 2] Patent No. 4373538 [Patent Document 3] JP 2006-196864 A Summary of the Invention

[0006] It is desirable to use an MMC plate as the cooling plate of an electrostatic chuck assembly because of its advantages of high thermal conductivity, low thermal expansion, etc. Therefore, there is a demand for improving the bonding strength in the bond between the MMC plate and the ceramic plate.

[0007] The inventors have now discovered that a bonded body of a ceramic plate and an MMC plate having high bonding strength can be provided by (1) providing a specified bonding layer between the MMC plate and the ceramic plate, and (2a) making the bonding interface between the ceramic plate and the bonding layer include an Mg-containing layer, and / or (2b) making the MMC plate have an Al diffusion layer extending to a specified depth (thickness) from the bonding interface between the bonding layer and the MMC plate.

[0008] SUMMARY OF THE PRESENT EMBODIMENTS Accordingly, an object of the present invention is to provide a joint of a ceramic plate and an MMC plate having high joint strength.

[0009] According to the present disclosure, the following aspects are provided. [Aspect 1] A ceramic plate and an MMC plate made of a metal matrix composite material (MMC) and disposed opposite one side of the ceramic plate; a bonding layer provided between the ceramic plate and the MMC plate for bonding the ceramic plate and the MMC plate, the bonding layer containing Al as a main component and Si and Mg as subcomponents; wherein the bonding interface between the ceramic plate and the bonding layer includes a Mg-containing layer. zygote. [Aspect 2] 2. The joined article of claim 1, wherein the Mg-containing layer further comprises Al and O. [Aspect 3] 3. The joined body according to aspect 2, wherein the weight ratio of Al:Mg:O in the Mg-containing layer is 1:0.01-0.50:0.001-0.100. [Aspect 4] Aspect 1, in which the Mg-containing layer has a thickness of 1 to 10 μm. ~One of 3 The conjugate according to claim 1, [Aspect 5] The bonding of the ceramic plate, the bonding layer, and the MMC plate is performed by thermal compression bonding. 4 13. The conjugate according to claim 12, [Aspect 6] The MMC comprises Si, C, and Ti. 5 13. The conjugate according to claim 12, [Aspect 7] The MMC plate is disposed at a predetermined depth D from the bonding interface between the bonding layer and the MMC plate. Al The embodiment 1 to 3 have an Al diffusion layer in which Al originating from the bonding layer is diffused throughout the entire surface of the substrate. 6 13. The conjugate according to claim 12, [Aspect 8] The MMC plate is disposed at a predetermined depth D from the bonding interface between the bonding layer and the MMC plate. Mg 8. The joined body according to claim 7, further comprising an Mg diffusion layer in which Mg derived from the joining layer is diffused throughout the joined body. [Aspect 9] The depth D of the Al diffusion layer Al is the depth D of the Mg diffusion layer Mg greater than D Al >D Mg The conjugate according to embodiment 8, which satisfies the above formula: [Aspect 10] The joined body according to any one of aspects 1 to 9, wherein the surface of the MMC plate at the joining interface side has an arithmetic mean roughness Ra of 0.01 to 1.0 μm. [Aspect 11] A bonded structure according to any one of aspects 1 to 10, which exhibits a bond strength of 200 MPa or more in a four-point bending test. [Aspect 12] 12. The joined body according to any one of aspects 1 to 11, wherein the ceramic plates contain aluminum oxide and / or aluminum nitride and have internal electrodes embedded therein. [Aspect 13] A ceramic plate and an MMC plate provided opposite one side of the ceramic plate and made of a metal matrix composite material (MMC) containing Si, C, and Ti; a bonding layer provided between the ceramic plate and the MMC plate for bonding the ceramic plate and the MMC plate, the bonding layer containing Al as a main component and Si and Mg as subcomponents; and the MMC plate is disposed at a predetermined depth D from a bonding interface between the bonding layer and the MMC plate. Al The Al diffusion layer has an Al diffusion layer in which Al originating from the bonding layer is diffused over a depth D Al The conjugate, wherein the diameter is 40 μm or more. [Aspect 14] The MMC plate is disposed at a predetermined depth D from the bonding interface between the bonding layer and the MMC plate. Mg14. The joined body according to claim 13, further comprising an Mg diffusion layer in which Mg derived from the joining layer is diffused throughout the joined body. [Aspect 15] The depth D of the Al diffusion layer Al is the depth D of the Mg diffusion layer Mg greater than D Al >D Mg The conjugate according to embodiment 14, wherein [Aspect 16] 16. The joined body according to any one of aspects 13 to 15, wherein the ceramic plates contain aluminum oxide and / or aluminum nitride and have internal electrodes embedded therein. [Aspect 17] 17. The joined body according to any one of aspects 13 to 16, wherein the ceramic plate, the joining layer, and the MMC plate are joined by thermocompression bonding. [Aspect 18] 18. The joined body according to any one of aspects 13 to 17, wherein the surface of the MMC plate at the joining interface side has an arithmetic mean roughness Ra of 0.01 to 1.0 μm. [Aspect 19] A bonded structure according to any one of aspects 13 to 18, which exhibits a bond strength of 200 MPa or more in a four-point bending test. [Brief description of the drawings]

[0010] [Figure 1] FIG. 1 is a schematic cross-sectional view showing an example of a bonded body according to the present invention. [Diagram 2] FIG. 4 is a schematic cross-sectional view showing another example of a bonded body according to the present invention. [Figure 3A] 1 shows an SEM image (Compo image) of a cross section including the ceramic plate 12, the bonding interface 20 and the bonding layer 16 in the bonded body of Example 7, and Si, C and Ti mapping images of the corresponding area. [Figure 3B] 1 shows an SEM image (Compo image) of a cross section including the ceramic plate 12, the bonding interface 20 and the bonding layer 16 in the bonded body of Example 7, and O, Mg and Al mapping images of the corresponding region. [Figure 4A]1 shows an SEM image (Compo image) of a cross section including the bonding layer 16, the bonding interface 22, and the MMC plate 14 in the bonded body of Example 7, and Si, C, and Ti mapping images of the corresponding area. [Figure 4B] 1 shows an SEM image (Compo image) of a cross section including the bonding layer 16, the bonding interface 22, and the MMC plate 14 in the bonded body of Example 7, and O, Mg, and Al mapping images of the corresponding region. [Figure 5A] 1 shows a SEM image (Compo image) of a cross section including the bonding layer 16, the bonding interface 22, and the MMC plate 14 in the bonded structure of Example 7, and reduced concentration scale versions of Si, C, and Ti mapping images of the corresponding area. [Figure 5B] 1 shows a SEM image (Compo image) of a cross section including the bonding layer 16, the bonding interface 22, and the MMC plate 14 in the bonded body of Example 7, and reduced concentration scale versions of O, Mg, and Al mapping images of the corresponding area. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0011] zygote FIG. 1 shows an example of a joined body according to the present invention. The joined body 10 shown in FIG. 1 includes a ceramic plate 12, an MMC plate 14, and a bonding layer 16. Preferably, the ceramic plate 12 includes aluminum oxide and / or aluminum nitride, and an internal electrode 18 is embedded in the ceramic plate 12. The MMC plate 14 is a plate made of a metal matrix composite material (MMC) and is provided facing one side of the ceramic plate 12. The metal matrix composite material (MMC) preferably includes Si, C, and Ti. The bonding layer 16 is a layer that bonds the ceramic plate 12 and the MMC plate 14, and is provided between the ceramic plate 12 and the MMC plate 14. The bonding layer 16 includes Al as a main component, and Si and Mg as subcomponents. In a first embodiment of the present invention, a bonding interface 20 between the ceramic plate 12 and the bonding layer 16 includes an Mg-containing layer 24. On the other hand, in a second embodiment of the present invention, as shown more specifically in FIG. 2, the MMC plate 14 is formed at a predetermined depth D from the bonding interface 22 between the bonding layer 16 and the MMC plate 14. Al The Al diffusion layer 26 is formed by diffusing Al originating from the bonding layer 16 over a depth D Al is preferably 40 μm or more. The first embodiment may include the features of the second embodiment, and vice versa. In this manner, by (1) providing a predetermined bonding layer 16 between the MMC plate 14 and the ceramic plate 12, and (2a) making the bonding interface 20 between the ceramic plate 12 and the bonding layer 16 include the Mg-containing layer 24, and / or (2b) making the MMC plate 14 have an Al diffusion layer 26 from the bonding interface 22 between the bonding layer 16 and the MMC plate 14 to a predetermined depth (thickness), a bonded body 10 of the ceramic plate 12 and the MMC plate 14 having high bonding strength can be provided. That is, by not only adopting the predetermined bonding layer 16 but also providing the Mg-containing layer 24 and / or the Al diffusion layer 26, a high bonding strength can be realized between the MMC plate 14 and the ceramic plate 12.

[0012] The ceramic plate 12 is a plate-shaped member including a ceramic sintered body, and may have the same configuration as a ceramic plate employed in a known ceramic susceptor (for example, an electrostatic chuck assembly, a ceramic heater, etc.). Typically, an internal electrode 18 is embedded in the ceramic plate 12. The ceramic sintered body constituting the main portion of the ceramic plate 12 other than the internal electrode 18 (i.e., the ceramic base) preferably contains aluminum oxide and / or aluminum nitride, more preferably aluminum nitride, from the viewpoints of excellent thermal conductivity, high electrical insulation, and thermal expansion characteristics similar to those of silicon. The ceramic sintered body constituting the ceramic plate 12 may contain additives such as MgO in addition to aluminum oxide and / or aluminum nitride. In this case, the content of aluminum oxide and / or aluminum nitride in the ceramic sintered body constituting the ceramic plate 12 is typically 50 to 100 mass %, and the remainder may contain additives such as MgO. The thickness of the ceramic plate 12 may be the thickness of a general ceramic plate, and is not particularly limited, but may be typically 2 to 10 mm, and more typically 2 to 5 mm.

[0013] Examples of the internal electrode 18 embedded in the ceramic plate 12 include an ESC electrode, a heater electrode, and an RF electrode. Two types of internal electrodes 18 may be provided in the ceramic plate 12. The ESC electrode is an abbreviation of an electrostatic chuck (ESC) electrode, and is also called an electrostatic electrode. The ESC electrode is preferably a circular thin-layer electrode having a diameter slightly smaller than that of the ceramic plate 12, and may be, for example, a mesh-like electrode formed by weaving thin metal wires into a net shape into a sheet shape. The ESC electrode may be used as a plasma electrode. That is, by applying a high frequency to the ESC electrode, the ESC electrode can also be used as a plasma electrode, and film formation can also be performed by a plasma CVD process. When a voltage is applied to the ESC electrode by an external power source, the ESC electrode chucks a wafer placed on the surface of the ceramic plate 12 by the Johnsen-Rahbek force. The heater electrode is not particularly limited, and may be, for example, a conductive coil wired in a single stroke over the entire surface of the ceramic plate 12. When power is supplied from the heater power supply, the heater electrode generates heat and heats the wafer placed on the surface of the ceramic plate 12. The heater electrode is not limited to a coil, and may be, for example, a ribbon (a long, thin plate) or a mesh. The ribbon-shaped heater electrode may be formed by a printing method.

[0014] The MMC plate 14 is made of a metal matrix composite (Metal Matrix Composite (MMC)). The MMC may be a known material in which a ceramic reinforcing material is composited in a metal matrix, and is not particularly limited. Examples of the metal matrix include aluminum and metal silicon. Examples of the ceramic reinforcing material include SiC and TiC. A preferred MMC includes Si, C, and Ti. An example of an MMC including Si, C, and Ti includes a composite material that contains 37 to 60 mass% of silicon carbide, and contains titanium silicon carbide and titanium carbide in amounts less than the content (mass%) of silicon carbide. The thickness of the MMC plate 14 is not particularly limited, but is typically 5 to 35 mm.

[0015] The surface of the MMC plate 14 on the bonding interface 22 side preferably has an arithmetic mean roughness Ra of 0.01 to 1.0 μm, and more preferably 0.05 to 0.70 μm. When the arithmetic mean roughness Ra is within the above range, the bonding strength can be more effectively increased. This is believed to be because Ra is not too high, which improves the adhesion between the MMC plate 14 and the bonding layer 16, and because Ra is not too low, which provides an anchor effect due to the surface roughness or unevenness of the MMC plate 14.

[0016] The bonding layer 16 is a metal layer containing Al as a main component and Si and Mg as secondary components. Here, the "main component" means a component that occupies 80% or more by weight of the bonding layer 16. The "secondary component" means a component (excluding inevitable impurities) that is contained in a lower amount than the main component. Therefore, the bonding material constituting the bonding layer 16 is preferably an Al alloy containing Si and Mg. The Si content of this Al alloy is preferably 5 to 15% by weight. Moreover, the Mg content of this aluminum alloy is preferably 0.1 to 5.0% by weight. That is, the bonding layer 16 is preferably composed of an Al alloy containing 5 to 15% by weight of Si and 0.5 to 5.0% by weight of Mg, with the remainder being Al alloy containing Al and inevitable impurities.

[0017] The bonding interface 20 between the ceramic plate 12 and the bonding layer 16 preferably includes an Mg-containing layer 24. The presence of the Mg-containing layer 24 at the bonding interface 20 improves the bonding strength between the ceramic plate 12 and the bonding layer 16, and as a result, it is believed that a high bonding strength can be realized between the ceramic plate 12 and the MMC plate 14. The Mg-containing layer 24 is identified as a layer containing Mg at a higher concentration than the surrounding area at the bonding interface 20 in an element mapping image obtained by EPMA (electron probe microanalyzer). The Mg-containing layer 24 preferably further contains Al and O. In this case, the weight ratio of Al:Mg:O in the Mg-containing layer 24 is preferably within the range of 1:0.01-0.50:0.001-0.100, and more preferably within the range of 1:0.05-0.30:0.005-0.050. The weight ratio of Al:Mg:O can be measured by EPMA. From the viewpoint of improving the bonding strength, the thickness of the Mg-containing layer 24 is preferably 1 to 10 μm, and more preferably 1 to 7 μm.

[0018] The ceramic plate 12, the bonding layer 16, and the MMC plate 14 are preferably bonded by thermocompression bonding. Thermocompression bonding is a method in which a metal bonding film (corresponding to the bonding layer 16) is sandwiched between two members to be bonded, and the two members are pressure-bonded while being heated to a temperature below the liquidus temperature of the metal bonding film (see Patent Document 1).

[0019] The MMC plate 14 is bonded to a predetermined depth D from the bond interface 22 between the bonding layer 16 and the MMC plate 14, as shown in FIG. AlIt is preferable that the MMC plate 14 has an Al diffusion layer 26 in which Al originating from the bonding layer 16 is diffused throughout the entire area. As described above, by providing the Al diffusion layer 26, a high bonding strength can be achieved between the MMC plate 14 and the ceramic plate 12. The Al diffusion layer 26 is identified as a layer containing Al at a higher concentration (than other areas of the MMC plate 14) observed in an Al element mapping image acquired by EPMA, as exemplified in FIG. 5B described later. That is, when pixels showing a high concentration of Al are distributed continuously from the bonding layer 16 over an area adjacent to the bonding interface 22 of the MMC plate 14 in the Al element mapping image, it can be said that the Al observed at a high concentration in the adjacent area of ​​the MMC plate 14 is Al originating from the bonding layer 16. In this way, the Al diffusion layer 26 is identified. The depth D of the Al diffusion layer 26 is determined by the following equation. Al The thickness is preferably 40 μm or more, more preferably 40 to 600 μm, further preferably 50 to 500 μm, and particularly preferably 250 to 500 μm.

[0020] As shown in FIG. 2, in addition to the Al diffusion layer 26, the MMC plate 14 has a predetermined depth D MgIt is preferable that the MMC plate 14 also has an Mg diffusion layer 28 in which Mg originating from the bonding layer 16 is diffused throughout the entire MMC plate 14. In this case, the Al diffusion layer 26 and the Mg diffusion layer 28 at least partially overlap each other (i.e., the MMC plate 14 has portions corresponding to both the Al diffusion layer 26 and the Mg diffusion layer 28). It is considered that the Mg diffusion layer 28, together with the Al diffusion layer 26, can contribute to realizing high bonding strength. The Mg diffusion layer 28 is identified as a layer containing Mg at a higher concentration (than other regions of the MMC plate 14) observed in a region adjacent to the bonding interface 22 of the MMC plate 14 in an Mg element mapping image obtained by EPMA, as exemplified in FIG. 5B described later. That is, when pixels showing a high concentration of Mg are distributed continuously from the bonding layer 16 over a region adjacent to the bonding interface 22 of the MMC plate 14 in the Mg element mapping image, it can be said that the Mg observed at a high concentration in the adjacent region of the MMC plate 14 is Mg originating from the bonding layer 16. In this way, the Mg diffusion layer 28 is identified. Depth D of Mg diffusion layer 28 Mg The depth D of the Al diffusion layer 26 is preferably 10 to 300 μm, more preferably 20 to 200 μm, and further preferably 90 to 180 μm. Al is the depth D of the Mg diffusion layer 28 Mg (i.e., D Al >D Mg (Meet the above requirements).

[0021] The MMC plate 14 may have an internal space, such as a flow path through which a coolant can flow, making the MMC plate 14 suitable for use as a cooling plate for an electrostatic chuck assembly.

[0022] The bonded body 10 exhibits a bond strength of preferably 200 MPa or more, more preferably 250 MPa or more, and even more preferably 300 MPa or more in a four-point bending test. The four-point bending test is performed according to the procedure and conditions disclosed in the examples described later, and the maximum bending stress obtained thereby is adopted as the bond strength. Since a high bond strength is desired, the upper limit is not particularly limited, but is typically 500 MPa or less, more typically 450 MPa or less.

[0023] Manufacturing method of the joint body The bonded body of the present invention may be produced by any method as long as a bonded body having a predetermined layer structure can be obtained, but a preferred production method will be described below.

[0024] First, the ceramic plate with the internal electrodes embedded, the MMC plate, and the bonding layer are prepared. The details of each component are as described above. The ceramic plate, the MMC plate, and the bonding layer may be any known material, or may be manufactured appropriately based on a known method.

[0025] Next, the ceramic plate, the MMC plate, and the bonding layer are each subjected to ultrasonic cleaning using an organic solvent. The ultrasonic cleaning can remove dirt adhering to the surface of each member, improve the bonding between each member and the bonding layer, and as a result, a high bonding strength can be realized. Preferred examples of the organic solvent include acetone and isopropyl alcohol (IPA). By increasing the ultrasonic cleaning time, dirt can be further removed, and the movement and diffusion of elements such as Mg and Al can be promoted during thermocompression bonding. Therefore, by controlling the ultrasonic cleaning time, it is possible to control the formation / non-formation of the Mg-containing layer in the subsequent thermocompression bonding, and to change the depth (thickness) of the Al diffusion layer and the depth (thickness) of the Mg-containing layer. For example, by increasing the ultrasonic cleaning time, it is possible to form the Mg-containing layer and increase the depth of the Al diffusion layer and the depth of the Mg-containing layer. From the viewpoint of more effectively removing dirt adhering to the surface of each member, it is desirable to perform both ultrasonic cleaning using acetone and ultrasonic cleaning using isopropyl alcohol (IPA). The ceramic plate and the MMC plate subjected to ultrasonic cleaning are washed with running pure water, washed with N 2 It is preferable to further clean the bonding layer by blowing with gas, wiping with a wipe sheet impregnated with an organic solvent (IPA, etc.), and drying. 2 It is preferable for the material to be further cleaned by blowing with a gas.

[0026] The ceramic plate, MMC plate, and bonding layer thus cleaned are used to prepare a bonded body by thermocompression bonding. For example, the bonding layer is sandwiched between the ceramic plate and the MMC plate, and while heating to a temperature lower than the liquidus temperature of the bonding material film, thermocompression bonding is performed at a pressure of 4 MPa to 30 MPa to bond the ceramic plate and the MMC plate via the bonding layer. The thermocompression bonding temperature is preferably lower than the liquidus temperature of the bonding layer and is equal to or higher than a temperature lower than the solidus temperature by about 30°C. For example, the liquidus temperature of an aluminum alloy containing 10% by weight of Si and 1% by weight of Mg is about 590°C, and the solidus temperature is about 560°C. Therefore, it can be said that the thermocompression bonding temperature in this case is preferably in the range of about 520°C or higher and lower than about 540°C. In this way, the bonded body of the present invention in which the ceramic plate and the MMC plate are bonded via the bonding layer can be obtained. EXAMPLES

[0027] The present invention will be described in more detail with reference to the following examples, although the present invention is not limited to the following examples.

[0028] Examples 1-9 (1) Preparation of ceramic plate As the ceramic plate, a disk-shaped aluminum oxide sintered body (thickness: 5 mm, diameter: 300 mm) in which the ESC electrodes were embedded was manufactured as follows. First, disk-shaped first and second green sheets made of alumina were prepared. The ESC electrodes were formed on one surface of the first green sheet by screen printing, while the heater electrodes were formed on one surface of the second green sheet by screen printing. Next, another alumina green sheet (hereinafter referred to as a third green sheet) was laminated on the surface of the first green sheet on which the ESC electrodes were formed, and the second green sheet was laminated thereon so that the heater electrodes were in contact with the third green sheet. The obtained laminate was fired by a hot press method to obtain a ceramic sintered body in which the ESC electrodes and the heater electrodes were embedded. The shape and thickness were adjusted by performing grinding, blasting, and the like on both surfaces of the obtained ceramic sintered body, and a flat-plate-shaped electrostatic chuck was obtained as a ceramic plate. Specific manufacturing conditions of this electrostatic chuck were set with reference to the conditions described in JP2006-196864A.

[0029] (2) Preparation of MMC plates As the MMC plate, a plate containing Si, C and Ti (SiSiCTi plate) was produced as follows. First, as raw materials, a SiC raw material (commercial product with a purity of 97% or more and an average particle size of 15.5 μm), a metal Si raw material (commercial product with a purity of 97% or more and an average particle size of 9.0 μm), and a metal Ti raw material (commercial product with a purity of 99.5% or more and an average particle size of 31.1 μm) were prepared. The SiC raw material, the metal Si raw material, and the metal Ti raw material were weighed to have a blend ratio of SiC: 49.5 mass%, Si: 20.0 mass%, and Ti: 30.5 mass%, and were put into a nylon pot together with isopropyl alcohol as a solvent, and wet-mixed for 4 hours using a nylon ball with an iron core having a diameter of 10 mm. The obtained slurry was taken out, dried at 110 ° C. in a nitrogen stream, and then passed through a 30-mesh sieve to obtain a blended powder. The blended powder was sieved at 200 kgf / cm 2The disk-shaped compact was then hot-pressed to obtain an MMC plate. The hot-press sintering was carried out in a vacuum atmosphere at a pressure of 200 kgf / cm. 2 The firing was performed by applying a pressing pressure of 1,400°C and maintaining the firing temperature (maximum temperature) at 1,400°C for 4 hours.

[0030] The arithmetic mean roughness Ra of the surface of the MMC plate thus prepared, to which the bonding layer was to be bonded, was measured using a stylus surface roughness tester in accordance with JIS B 0601-2001. The results are shown in Table 1.

[0031] (3) Preparation of the bonding layer A 0.12 mm thick Al alloy sheet containing Si and Mg (alloy composition: Si: 10 wt %, Mg: 1 wt %, balance: Al and unavoidable impurities) was prepared as a bonding layer.

[0032] (4) Cleaning process The ceramic plate and the MMC plate were subjected to the following cleaning steps (i) to (ii). v ) were sequentially performed on the Si- and Mg-containing Al alloy sheet, whereas the following cleaning steps (i), (ii) and (iv) alone were sequentially performed on the Si- and Mg-containing Al alloy sheet. <Cleaning process> (i) Ultrasonic cleaning with acetone (not performed in Example 9) (ii) Ultrasonic cleaning with isopropyl alcohol (IPA) (not performed in Example 9) (iii) Rinse with running pure water (iv)N 2 Gas blowing (v) Dry at 120°C for 10 minutes

[0033] At this time, the total cleaning time of (i) ultrasonic cleaning using acetone and (ii) ultrasonic cleaning using isopropyl alcohol (IPA), that is, the ultrasonic cleaning time with an organic solvent, was changed for each experimental example as shown in Table 1. Therefore, as described above, for Example 9, the ultrasonic cleaning of (i) and (ii) was not performed.

[0034] (5) Thermocompression bonding Thermocompression bonding was performed as follows using the cleaned ceramic plate, MMC plate, and bonding sheet, respectively. That is, a bonding sheet was sandwiched as a bonding layer between the ceramic plate and the MMC plate, and heated to 530 °C (a temperature lower than the liquidus temperature of the Si- and Mg-containing Al alloy and higher than a temperature about 30 °C lower than the solidus temperature), and then thermocompression bonded at a pressure of 20 MPa in a vacuum to bond the ceramic plate, the bonding sheet (bonding layer), and the MMC plate to each other. Thus, a bonded body in which the ceramic plate and the MMC plate were bonded via the bonding layer was obtained.

[0035] (6) Evaluation of the bonded body The following evaluations were performed on the fabricated bonded body.

[0036] <Obtaining an elemental mapping image by EPMA> A cross section of the obtained bonded body was cut out and mirror-polished, and then flat ion milling was performed with Ar ions to obtain an observation cross section. A 75 μm×75 μm region including the ceramic plate 12, the bonding interface 20, and the bonding layer 16 in the obtained observation cross section was observed with a SEM (scanning electron microscope), and elemental analysis was performed on the region with an EPMA (manufactured by JEOL Ltd.) at an acceleration voltage of 15 kV, to obtain elemental mapping images of Si, C, Ti, O, Mg, and Al. Figures 3A and 3B show SEM images (Compo images) of a cross section including the ceramic plate 12, the bonding interface 20, and the bonding layer 16 in the bonded body of Example 7, and various elemental mapping images of the corresponding regions. As a result, as shown in Table 1 and Figures 3A and 3B, in the bonded bodies of Examples 1 to 7, a Mg-containing layer 24 containing Mg at a higher concentration than the surrounding area was observed at the bonding interface 20, and it was also confirmed that this Mg-containing layer 24 further contained Al and O. On the other hand, in the joints of Examples 8 and 9 (Comparative Examples), such an Mg-containing layer was not observed.

[0037] In addition, the bonding layer 16, the bonding interface 22, and the MMC plate 14 in the obtained observation cross section of Similarly, SEM observation and EPMA elemental analysis were performed on a 75 μm × 75 μm region including the bonding layer 16, bonding interface 22, and MMC plate 14 in the bonded body of Example 7. Figures 4A and 4B show SEM images (Compo images) of a cross section including the bonding layer 16, bonding interface 22, and MMC plate 14 in the bonded body of Example 7, and elemental mapping images of the corresponding region. As a result, as shown in Figures 4A and 4B, in all of the bonded bodies of Examples 1 to 9, TiC particles (see black particles in the figure), TiSi 2 A microstructure having a matrix (see the gray part in the figure) and SiC particles (see the white particles in the figure) was observed. In addition, in the joints of Examples 1 to 7, it was also confirmed that Mg and Al were diffused into the SiSiCTi constituting the MMC plate 14.

[0038] Furthermore, the bonding layer 16, the bonding interface 22 and the MMC plate 14 ofFor a wider cross-sectional area of 300 μm × 300 μm including it, SEM observation and EPMA elemental analysis were performed in the same manner as above except that the magnification was lowered and the concentration scale was reduced. Figures 5A and 5B show a version with the concentration scale reduced of the SEM image (Compo image) of the cross-section including the bonding layer 16, the bonding interface 22, and the MMC plate 14 in the bonded body of Example 7 and the concentration scale of the various elemental mapping images of the corresponding regions. As a result, in the bonded bodies of Examples 1 to 9, the presence of an Al diffusion layer 26 and a Mg diffusion layer 28 in which Al and Mg derived from the bonding layer 16 were diffused over the depth direction of the MMC plate 14 from the bonding interface 22 were confirmed within the MMC plate 14. The depth D Al from the bonding interface 22 of the Al diffusion layer 26 Mg and the depth D

[0039] <Weight ratio of Al:Mg:O in the Mg-containing layer> From the EPMA measurement results, semi-quantitative values of each element for each pixel corresponding to 0.24 μm × 0.24 μm were calculated, and the weight ratio of Al:Mg:O was calculated by performing a weight ratio calculation from the average value of 300 pixels.

[0040] <Bonding strength> From the obtained bonded body, a long sample was cut out so that the bonding layer was located at the center in the longitudinal direction, and the surface of the sample was ground to produce a test piece having dimensions of 1.5 mm × 2.0 mm × 20 mm. A four-point bending test was performed on this test piece under the conditions of a lower span of 15 mm, an upper span of 5 mm, and a crosshead speed of 0.5 mm / min with the bonding interface at the center, and the obtained maximum bending stress (MPa) was taken as the bonding strength. The results were as shown in Table 1.

[0041]

Table 1

Claims

1. A ceramic plate containing aluminum oxide; an MMC plate provided opposite one side of the ceramic plate and made of a metal matrix composite material (MMC) containing Si, C, and Ti; a bonding layer provided between the ceramic plate and the MMC plate for bonding the ceramic plate and the MMC plate, the bonding layer containing Al as a main component and Si and Mg as subcomponents; wherein the bonding interface between the ceramic plate and the bonding layer includes a Mg-containing layer. zygote.

2. The joint body according to claim 1 , wherein the Mg-containing layer further comprises Al and O.

3. 3. The joined body according to claim 2, wherein the weight ratio of Al:Mg:O in the Mg-containing layer is 1:0.01-0.50:0.001-0.

100.

4. 3. The joined body according to claim 1, wherein the Mg-containing layer has a thickness of 1 to 10 μm.

5. The method for producing a joint body according to any one of claims 1 to 3, wherein the ceramic plate, the joint layer and the MMC plate are joined by thermocompression bonding.

6. The MMC plate is disposed at a predetermined depth D from the bonding interface between the bonding layer and the MMC plate. Ａｌ The joined body according to any one of claims 1 to 3, further comprising an Al diffusion layer in which Al originating from the joining layer is diffused throughout the joined body.

7. The MMC plate is disposed at a predetermined depth D from the bonding interface between the bonding layer and the MMC plate. Ｍｇ The joined body according to claim 6 , further comprising an Mg diffusion layer in which Mg derived from the joining layer is diffused throughout the joined body.

8. The depth D of the Al diffusion layer Ａｌ is the depth D of the Mg diffusion layer Ｍｇ That is, D Ａｌ >D Ｍｇ The composite according to claim 7, which satisfies the above formula.

9. The joint body according to any one of claims 1 to 3, wherein the surface of the MMC plate at the joining interface side has an arithmetic mean roughness Ra of 0.01 to 1.0 µm.

10. The bonded body according to any one of claims 1 to 3, which exhibits a bond strength of 200 MPa or more in a four-point bending test.

11. 4. The joined body according to claim 1, wherein the ceramic plate has an internal electrode embedded therein.

12. A ceramic plate comprising aluminum oxide; an MMC plate provided opposite one side of the ceramic plate and made of a metal matrix composite material (MMC) containing Si, C, and Ti; a bonding layer provided between the ceramic plate and the MMC plate for bonding the ceramic plate and the MMC plate, the bonding layer containing Al as a main component and Si and Mg as subcomponents; and the MMC plate is provided with a predetermined depth D from a bonding interface between the bonding layer and the MMC plate. Ａｌ The Al diffusion layer has an Al diffusion layer in which Al originating from the bonding layer is diffused over a depth D Ａｌ The bonded body, wherein the thickness is 40 μm or more.

13. The MMC plate is disposed at a predetermined depth D from the bonding interface between the bonding layer and the MMC plate. Ｍｇ The joined body according to claim 12, further comprising an Mg diffusion layer in which Mg derived from the joining layer is diffused throughout the joined body.

14. The depth D of the Al diffusion layer Ａｌ is the depth D of the Mg diffusion layer Ｍｇ is greater than D Ａｌ >D Ｍｇ The composite according to claim 13 ,

15. The joined body according to any one of claims 12 to 14, wherein the ceramic plate has an internal electrode embedded therein.

16. The method for producing a joint body according to any one of claims 12 to 14, wherein the ceramic plate, the joint layer and the MMC plate are joined by thermocompression bonding.

17. The joint body according to any one of claims 12 to 14, wherein the surface of the MMC plate at the joining interface side has an arithmetic mean roughness Ra of 0.01 to 1.0 μm.

18. The bonded body according to any one of claims 12 to 14, which exhibits a bond strength of 200 MPa or more in a four-point bending test.

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