Conjugate, method for producing the same, and electrode embedding member

Abstract

To provide a joined body which can suppress erosion and contamination of a joined surface, has strong bond strength, and has thick metal member, a method for manufacturing the same, and an electrode embedding member.SOLUTION: There is provided a joined body 10 of a ceramic member 20 containing AIN as a main component and a metal member 30 composed of high melting point metal having a melting point of 2,000°C or higher, wherein the ceramic member 20 is joined to at least one main surface 32 of the metal member 30, the ceramic member 20 includes a second phase composed of a metal oxide, the metal member 30 has a maximum thickness in a direction perpendicular to the one main surface 32 of the metal member 30 of 1 mm or more, and in a joint interface between the ceramic member 20 and the metal member 30, the concentration of metal constituting the second phase and oxygen concentration of the ceramic member 20 are larger than the concentration of the metal and the oxygen concentration inside the ceramic member 20.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to a joined body, a method for manufacturing the same, and an electrode embedding member.

Background Art

[0002] AlN members used in semiconductor manufacturing apparatuses have sometimes been joined to metal members for the purpose of adding various functions.

[0003] Patent Document 1 discloses a joined body in which an aluminum nitride member and a metal member are joined with an Al brazing material, and a semiconductor holding device. As a preferred embodiment, an example is disclosed in which the aluminum nitride member is a semiconductor holding member having an installation surface for installing a semiconductor wafer, and the metal member is a heat transfer member for transferring heat between the semiconductor holding member and the outside. Further, as an example of the heat transfer member, it is disclosed that it is formed of tungsten, molybdenum, copper, or an alloy thereof. These metal members function as heat sinks and have a certain thickness.

[0004] Further, Patent Document 2 aims to provide an aluminum nitride joined body and a method for manufacturing the same, which have a sintered metal layer having a relatively large thickness and high conductivity, and in which the occurrence of warpage is extremely small, and further, the joining strength between the sintered metal layer and the substrate is also high, and are suitable for use as an electrode embedding member. A joined body of an aluminum nitride sintered body in which a sintered metal layer made of tungsten or molybdenum having a thickness of 15 to 100 μm is formed on at least a part of the joining surface, and the sheet resistance value of the sintered metal layer is 1 Ω / square or less, and the warpage of the sintered metal layer is 100 μm / 100 mm or less is disclosed.

Prior Art Documents

Patent Documents

[0005]

Patent Document 1

Patent Document 2

[0006] [Non-Patent Document 1 Journal of the Japan Institute of Metals, Vol. 45, No. 2 (1981), pp. 184-189 [Summary of the Invention [Problems to be Solved by the Invention

[0007] AlN ceramics used in semiconductor manufacturing processes may be integrated with high melting point metals (metals with a melting point of 2000 °C or higher) such as heat sinks. For this purpose, the high melting point metal requires a certain thickness or more, but such a structure could not be achieved with a sintered metal layer as in Patent Document 2.

[0008] Also, according to Non-Patent Document 1, it has been considered difficult to fabricate a joined body because AlN and high melting point metals do not react without a joining material. Therefore, conventionally, a joined body of AlN ceramic and high melting point metal has been fabricated by a method of joining with an interposing brazing material or the like at the joining interface (Patent Documents 1, 3, and 4).

[0009] However, when these joined bodies are used in semiconductor manufacturing processes, in the methods of Patent Documents 1, 3, and 4, there are concerns about erosion of the brazing material as the joining layer and contamination from the joining layer. Therefore, there has been a demand for an AlN-high melting point metal joined body that is a joined body of AlN ceramic and a thick high melting point metal and suppresses the risk of contamination and erosion from the joining material.

[0010] The present invention has been made in view of such circumstances, and an object thereof is to provide a joined body that can suppress erosion and contamination of a joint surface, has high joint strength, and has a thick metal member, a method for manufacturing the same, and an electrode embedding member.

Means for Solving the Problems

[0011] (1) To achieve the above object, the joined body of the present invention is a joined body of a ceramic member mainly composed of AlN and a high melting point metal having a melting point of 2000 ° C or higher. Mo, W, or a Mo alloy as such It is characterized in that the ceramic member is joined to at least one main surface of the metal member, the ceramic member contains a second phase composed of 2 to 3 metal oxides, and the metal member has a maximum thickness in a direction perpendicular to one main surface of the metal member of 1 mm or more. The joint interface between the ceramic member and the metal member is characterized in that the concentration of the metal and the oxygen concentration constituting the second phase of the ceramic member are each higher than the concentration of the metal and the oxygen concentration inside the ceramic member. The ceramic member has electrodes embedded therein, The ceramic member is joined to at least one main surface of the metal member, the ceramic member contains a second phase composed of metal oxides 2 to 3, the metal member has a maximum thickness in a direction perpendicular to one main surface of the metal member of 1 mm or more, and the joint interface between the ceramic member and the metal member is characterized in that the concentration of the metal and the oxygen concentration constituting the second phase of the ceramic member are each higher than the concentration of the metal and the oxygen concentration inside the ceramic member. Y as such 2 O 3, the metal member has a maximum thickness in a direction perpendicular to one main surface of the metal member of 1 mm or more, and the joint interface between the ceramic member and the metal member is characterized in that the concentration of the metal and the oxygen concentration constituting the second phase of the ceramic member are each higher than the concentration of the metal and the oxygen concentration inside the ceramic member.

[0012] In this way, since the concentration of the metal and the oxygen concentration constituting the second phase of the joint interface between the ceramic member mainly composed of AlN and the metal member made of a high melting point metal are each higher than the concentration of the metal and the oxygen concentration inside the ceramic member, the ceramic member and the metal member are joined through these, and a joined body in which erosion and contamination of the joint surface are suppressed can be obtained. In addition, since the thickness of the metal member is large, it can be applied to various uses such as using the metal member as a heat sink or a heat spreader, or increasing the strength and dimensional accuracy of the ceramic member. If the maximum thickness of the metal member is less than 1 mm, the effect of improving the dimensional accuracy cannot be sufficiently exhibited, so it is preferably 1 mm or more.

[0013] (2) Further, in the joined body of the present invention, the ceramic member contains a Group 4 metal, and the metal member is characterized in that the Group 4 metal has diffused.

[0014] In this way, since the ceramic member contains a Group 4 metal and the Group 4 metal has diffused into the metal member, the bonding strength between the ceramic member and the metal member is increased, and the reliability of the bonded body is enhanced.

[0015] (3) Further, in the bonded body of the present invention, the metal member is characterized by containing 1 wt% or less of a second metal oxide.

[0016] In this way, since the metal member contains 1 wt% or less of the second metal oxide, the bonding strength between the ceramic member and the metal member is increased, and the reliability of the bonded body is enhanced.

[0017] (4) Further, the bonded body of the present invention is characterized in that a ceramic member is further bonded to the other main surface on the side facing one main surface of the metal member.

[0018] In this way, by bonding ceramic members to both main surfaces of the metal member, the applications of the bonded body are further expanded.

[0019] (5) Further, the electrode-embedded member of the present invention is characterized by including the bonded body according to any one of (1) to (3) above and an electrode embedded in the ceramic member of the bonded body.

[0020] Since AlN has high thermal conductivity and high insulation, an electrode-embedded member in which an electrode is embedded in the ceramic member of a bonded body of a ceramic member and a metal member can be used as a heater module having excellent thermal conductivity.

[0021] (6) Further, the method for manufacturing the bonded body of the present invention is a method for manufacturing a bonded body of a ceramic member mainly composed of AlN and a high melting point metal having a melting point of 2000°C or higher Mo, W, or a Mo alloy as such and a metal member, and a metal oxide is added to the AlN raw material powder Y as such 2 O 3 ofA step of granulating the powder added with the raw material powder to produce granulated powder, and laminating the granulated powder or a molded body formed from the granulated powder and a plate-shaped high melting point metal with a thickness of 1 mm or more in a carbon mold so that one main surface of the plate-shaped high melting point metal is perpendicular to the lamination direction, inserting a carbon punch into the carbon mold to form a laminate, A step of embedding electrodes in the molded body or laminating the electrodes on the carbon mold so as to sandwich the molded body therebetween; and a step of uniaxially pressure-sintering the laminate, and is characterized by including the above.

[0022] Thereby, a joined body of a ceramic member and a metal member with erosion and contamination of the joined surface suppressed can be obtained. Since the thickness of the metal member is large, it can be applied to various uses such as using the metal member as a heat sink or increasing the strength and dimensional accuracy of the ceramic member.

Effect of the Invention

[0023] According to the present invention, a joined body in which erosion and contamination of the joined surface of a ceramic member mainly composed of AlN and a metal member made of a high melting point metal are suppressed can be obtained. Further, since the thickness of the metal member is large, it can be applied to various uses such as using the metal member as a heat sink or increasing the strength and dimensional accuracy of the ceramic member.

Brief Description of the Drawings

[0024]

Figure 1

Figure 2

Figure 3

Figure 4

Figure 5

Mode for Carrying Out the Invention

[0025] 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 duplicate descriptions are omitted. In the configuration diagrams, the sizes of the respective components are conceptually represented and do not necessarily represent actual dimensional ratios.

[0026] [Embodiment] [Configuration of the Joined Body] First, a joined body according to an embodiment of the present invention will be described. FIG. 1 is a schematic cross-sectional view showing an example of a joined body according to an embodiment of the present invention. The joined body 10 according to an embodiment of the present invention is formed by joining a ceramic member 20 mainly composed of AlN and a metal member 30 made of a high melting point metal. The ceramic member mainly composed of AlN means that it contains 90 wt% or more of AlN. Also, the metal member made of a high melting point metal refers to those such as molybdenum (Mo), tungsten (W), tantalum (Ta), etc. having a melting point of 2000°C or higher, and those with a purity of 99 wt% or more. Thereby, deformation of the metal member 30 is suppressed even at the temperature during uniaxial pressure sintering. At the same time, since a high melting point metal oxide having a relatively high melting point of 900°C or higher is formed at the interface between AlN and the metal member 30, deformation of the joining interface between AlN and the metal member 30 can be suppressed.

[0027] In the joined body 10, the ceramic member 20 is joined to at least one main surface of the metal member 30. Also, the metal member 30 preferably has a maximum diameter of 50% or more of the maximum diameter of the ceramic member 20. Further, the ceramic member 20 is preferably joined to the entire surface of one main surface of the metal member 30. By having these characteristics, the metal member 30 can be applied in forms according to various uses. Also, the ceramic member 20 is preferably directly joined to one main surface of the metal member 30 without interposing another member. This is because if another member is interposed, the joining strength may be reduced.

[0028] The ceramic member 20 contains a second phase composed of a metal oxide. The metal constituting the metal oxide of the second phase is preferably at least one selected from Y and Ca, and more preferably Y. The metal oxide constituting the second phase may be a sintering aid for the ceramic member mainly composed of AlN. In that case, the metal oxide constituting the second phase may be added in an amount necessary as a sintering aid for the ceramic member. For example, when Y is added as a sintering aid, it may be added in an amount of 0.1 wt% or more and 5 wt% or less in terms of Y2O3 conversion.

[0029] The metal member 30 has a maximum thickness in a direction perpendicular to one main surface 32 of the metal member 30 of 1 mm or more. Thus, due to the large thickness of the metal member 30, it can be applied to various uses such as using the metal member 30 as a heat sink or a heat spreader, or increasing the strength and dimensional accuracy of the ceramic member 20. One main surface 32 of the metal member 30 is a joint surface with the ceramic member 20. The large thickness of the metal member 30 means that the maximum thickness in a direction perpendicular to one main surface 32 of the metal member 30 is 1 mm or more. If the maximum thickness of the metal member 30 is less than 1 mm, the effect of improving the dimensional accuracy cannot be sufficiently exhibited, so it is preferably 1 mm or more.

[0030] The maximum thickness in a direction perpendicular to one main surface 32 of the metal member 30 is preferably set to a thickness according to the application. Considering that there was no joined body with a large thickness of the metal member 30 as in the present invention, depending on the application, for example, it is preferably 2 mm or more, more preferably 3 mm or more, and even more preferably 4 mm or more.

[0031] The bonding interface between the ceramic member 20 and the metal member 30 is such that the concentration of the metal and the oxygen concentration that constitute the second phase of the ceramic member 20 are each greater than the concentration of the metal and the oxygen concentration inside the ceramic member 20. Thus, since the concentration of the metal and the oxygen concentration that constitute the second phase of the bonding interface between the ceramic member 20 mainly composed of AlN and the metal member 30 made of a high melting point metal are each greater than the concentration of the metal and the oxygen concentration inside the ceramic member 20, the ceramic member 20 and the metal member 30 are bonded through these, and a bonded body with suppressed erosion and contamination of the bonding surface is obtained.

[0032] Note that the bonding interface between the ceramic member 20 and the metal member 30 refers to the interface where the metal element mainly constituting the metal member 30 rapidly decreases its concentration in the cross-sectional element mapping by EDX or EPMA. Also, the inside of the ceramic member 20 refers to a region that is at least 1 mm away from the bonding interface and where the concentration of the metal that constitutes the second phase of the ceramic member 20 is uniform.

[0033] The change in the concentration of the metal present in the ceramic member 20, the metal member 30, or their bonding interface can be determined by comparing the intensity (count number) of the characteristic X-rays of the region by EPMA. Thereby, the difference in the metal and oxygen concentrations near the interface and inside can be relatively evaluated.

[0034] The ceramic member 20 preferably further contains a Group 4 metal, and it is preferable that the Group 4 metal has diffused into the metal member 30. Thus, since the ceramic member 20 contains a Group 4 metal and the Group 4 metal has diffused into the metal member 30, the bonding strength between the ceramic member 20 and the metal member 30 is increased, and the reliability of the bonded body 10 is enhanced. The Group 4 metal is preferably one or more selected from Ti and Hf, and more preferably Ti.

[0035] The metal member 30 preferably contains 1 wt% or less of the second metal oxide. By the metal member 30 containing 1 wt% or less of the second metal oxide, the bonding strength between the ceramic member 20 and the metal member 30 is increased, and the reliability of the bonded body 10 is enhanced. The metal constituting the second metal oxide is preferably at least one selected from Y, Ce, and Ca, and more preferably Y or Ce. The metal constituting the second metal oxide may be the same as the metal constituting the metal oxide of the second phase of the ceramic member 20. These metal oxide components pre - contained in the metal member 30 can increase the metal and oxygen concentrations at the bonding interface and enhance the bonding strength.

[0036] Figure 2 is a schematic cross - sectional view showing a modified example of the bonded body according to an embodiment of the present invention. As shown in Figure 2, it is preferable that the ceramic member 20 is further bonded to the other main surface 34 on the side facing one main surface 32 of the metal member 30. Thus, by bonding the ceramic member 20 to both main surfaces of the metal member 30, the applications of the bonded body 10 are further expanded. Also, by sandwiching the plate - shaped high - melting - point metal (metal member 30) with the ceramic member 20, warping of the bonded body 10 can be suppressed, and a bonded body 10 with high dimensional accuracy can be produced. Note that one main surface 32 and the other main surface 34 together are referred to as both main surfaces 32, 34 or main surfaces 32, 34. Also, the ceramic member 20 may be bonded to a surface of the bonded body 10 other than the main surfaces 32, 34.

[0037] [Configuration of Electrode - Embedded Member] Next, the electrode - embedded member according to an embodiment of the present invention will be described. Figure 3 is a schematic cross - sectional view showing an example of the electrode - embedded member according to an embodiment of the present invention. The electrode - embedded member 50 according to an embodiment of the present invention includes the bonded body 10 and an electrode 40 embedded in the ceramic member 20 of the bonded body 10.

[0038] The joined body 10 is the above-described joined body 10. The electrode 40 is embedded in the ceramic member 20 of the joined body 10. The shape of the electrode 40 can be various shapes such as a mesh shape or a foil shape. Also, the material can be various materials such as molybdenum and tungsten. The electrode 40 can be used as an electrode for a heater.

[0039] The electrode embedding member 50 may be provided with terminal holes and terminals (not shown).

[0040] The joined body and the electrode embedding member of the present invention are members that suppress erosion and contamination of the joint surface between a ceramic member mainly composed of AlN and a metal member made of a high melting point metal. Also, the joined body and the electrode embedding member of the present invention can be applied to various uses such as utilizing the metal member as a heat sink or a heat spreader due to the thickness of the metal member being thick, or enhancing the strength and dimensional accuracy of the ceramic member.

[0041] [Method for manufacturing the joined body] Next, a method for manufacturing the joined body 10 configured as described above will be described. FIGS. 4(a) to (e) are cross-sectional views schematically showing one step of the manufacturing process of the manufacturing method according to the embodiment of the present invention.

[0042] First, a powder obtained by adding a metal oxide raw material powder to an AlN raw material powder is granulated to produce granulated powder 22. The AlN raw material powder is preferably of high purity, and its purity is preferably 96% or more, more preferably 98% or more. Also, the average particle size of the AlN powder is preferably 0.1 μm or more and 1.0 μm or less, more preferably 0.3 μm or more and 0.8 μm or less. When, for example, Y2O3 is used as the metal oxide raw material powder, 0.1 wt% to 5 wt% of Y2O3 is added to the AlN raw material powder in an internal ratio, and a binder such as a PVA-based binder, a dispersant, and a solvent are added to prepare a slurry, and the granulated powder 22 is granulated by a spray dryer or the like.

[0043] Next, prepare a plate-shaped high melting point metal 36 with a thickness of 1 mm or more, and stack the granulated powder 22 or the formed body formed from the granulated powder and the plate-shaped high melting point metal 36 with a thickness of 1 mm or more in a bottomed carbon mold 60 (forming mold) such that one main surface of the plate-shaped high melting point metal 36 is perpendicular to the stacking direction.

[0044] As another example of stacking the formed bodies, one or more formed bodies are produced using the obtained granulated powder 22. As the forming method of the formed body, for example, known methods such as uniaxial pressing or cold isostatic pressing (CIP) method may be used. Note that the method of forming the formed body is not limited to pressure forming, and for example, green sheet lamination or casting molding is also applicable.

[0045] When producing the electrode embedding member 50, when stacking the granulated powder 22, the granulated powder 22 is temporarily pressed, the electrode 40 is disposed, further granulated powder 22 is introduced and temporarily pressed, or the formed bodies are stacked, the electrode 40 is disposed, and further formed bodies are stacked, so that the electrode 40 is embedded in the portion that becomes the ceramic member 20 after sintering.

[0046] Next, insert a carbon punch 70 into the carbon mold 60 to form a laminate 12. The laminate 12 may be composed of two layers, namely, a layer of the granulated powder 22 or the formed body that becomes the ceramic member 20 after sintering and a plate-shaped high melting point metal 36 that becomes the metal member 30 after sintering, or may be composed of three layers in which the plate-shaped high melting point metal 36 is sandwiched between layers of the granulated powder 22 or the formed body. Also, on the side surface in the stacking direction, there may be a portion where the plate-shaped high melting point metal 36 is exposed, or the plate-shaped high melting point metal 36 may be covered with the granulated powder 22 or the formed body. FIG. 4 shows a case where the plate-shaped high melting point metal 36 is covered with the granulated powder 22 and produced in three layers.

[0047] Next, the joined body 10 is produced by uniaxially pressure-sintering the laminate 12. The sintering conditions can be, for example, sintering by holding at a temperature of 1700 °C or higher and 2000 °C or lower and a pressure of 1 MPa or higher for 0.1 hour or more and 10 hours or less.

[0048] After firing, a step of processing into a predetermined shape may be provided. At this time, when the side surface in the stacking direction of the plate-shaped high melting point metal 36 is covered with the ceramic member, processing may be performed to expose the plate-shaped high melting point metal 36. Further, when the plate-shaped high melting point metal 36 is a three-layer structure sandwiched between the layers of the ceramic member 20, processing may be performed to remove a part of the ceramic member 20 or all of one of the ceramic members 20. Further, a step of processing the shape of the plate-shaped high melting point metal 36 may be provided. At this time, the processing is performed so that the maximum thickness in the direction perpendicular to one main surface 32 of the plate-shaped high melting point metal 36 does not fall below 1 mm.

[0049] Further, when the electrode embedding member 50 is used, a step of exposing a part of the electrode 40 or a step of connecting a terminal to the electrode 40 may be provided.

[0050] In addition, in the method of manufacturing and stacking the formed body, a step of degreasing the formed body to produce a degreased body and a step of pre-firing the degreased body to produce a pre-fired body may be provided. In that case, for example, the degreasing temperature is preferably 400°C or higher and 800°C or lower, and the degreasing time is preferably 1 hour or longer and 120 hours or shorter. The degreasing atmosphere is preferably an air atmosphere or a nitrogen atmosphere, and more preferably an air atmosphere. Further, for example, the pre-firing temperature is preferably 1200°C or higher and 1700°C or lower, and the pre-firing time is preferably 0.5 hour or longer and 12 hours or shorter. The pre-firing atmosphere is preferably a nitrogen or inert gas atmosphere, but may also be an atmosphere such as vacuum.

[0051] By such a method, a joined body or an electrode embedding member in which erosion and contamination of the joining surface between the ceramic member mainly composed of AlN and the metal member made of a high melting point metal are suppressed can be manufactured.

[0052] [Examples] (Manufacture of joined body) (Example 1) 5 wt% of Y2O3 was added to the AlN raw material powder based on the internal ratio, and a binder (PVA), a dispersant, and a solvent were added to prepare a slurry, and the granulated powder was granulated by a spray dryer. Also, as a plate-shaped high-melting-point metal to be a metal member, Mo with a diameter of Φ50 mm and a thickness of 5 mm was prepared.

[0053] Next, the granulated powder was filled into a carbon mold with a bottom, and press-molded with a carbon punch to produce a molded body with a diameter of Φ80 mm and a thickness of 10 mm. Next, Mo was placed on the molded body. Next, the granulated powder was further filled into the carbon mold to embed Mo. At this time, filling of the granulated powder and molding with a carbon punch were performed so that the thickness from the upper surface of Mo became 10 mm.

[0054] Then, with the carbon punch inserted into the carbon mold, uniaxial hot press sintering was performed at a temperature of 1800 °C, a pressure of 4 MPa, and in an N2 atmosphere for 2 hours. As a result, a metal member made of Mo with a diameter of 50 mm could be embedded inside the AlN sintered body with a diameter of 80 mm. In this way, the joined body of Example 1 was produced. After that, a plurality of test pieces of Example 1 with dimensions of 3 mm × 4 mm × 19 mm were cut out so that the stacking direction became the long side.

[0055] (Example 2) The joined body of Example 2 was produced under the same process and conditions, except that the granulated powder of Example 1 was changed to one in which 5 wt% of Y2O3 and 0.9 wt% of TiN were added to the AlN raw material powder based on the internal ratio.

[0056] (Example 3) The joined body of Example 3 was produced under the same process and conditions, except that the high-melting-point metal of Example 1 was replaced with an alloy in which 0.4 wt% of Y2O3 was added to Mo.

[0057] (Example 4) The joined body of Example 4 was produced under the same process and conditions, except that the high-melting-point metal of Example 1 was replaced with W.

[0058] (Measurement of joining strength) The three-point bending strength test was carried out in accordance with JIS R1601 2008 (Test method for room temperature bending strength of fine ceramics) to measure the bonding strength of the bonded body. The span was set to 10 mm, and the bonding surface was placed at the central part in the longitudinal direction, and the measurement was carried out with the knife edge aligned with the bonding surface. Five test pieces were prepared for each sample, and the average value of the five measured values was taken as the bonding strength value of each sample.

[0059] (Measurement results) In Example 1, the bonding strength was 77 MPa, and in Example 4, it was 90 MPa, indicating that sufficient bonding strength was obtained. In Example 2, the bonding strength was 115 MPa, and a higher bonding strength than that of the sample in Example 1 was obtained. Also, in Example 3, it was 103 MPa, and a higher bonding strength than that of the sample in Example 1 was obtained.

[0060] (Example 5) (Fabrication of electrode embedding member) In Example 5, a heater electrode was embedded in the AlN sintered body (ceramic member) located above Mo in the manufacturing method of Example 1 to fabricate a heater module that can be used in a high-temperature process.

[0061] The granulated powder was prepared in the same manner as in Example 1. Also, as the plate-shaped high-melting-point metal that becomes the metal member, a plate-shaped Mo with a diameter of Φ300 mm and a thickness of 8 mm was prepared.

[0062] First, a heater laminate was fabricated. The granulated powder was filled into a bottomed carbon mold and press-molded with a carbon punch to fabricate a molded body with a diameter of Φ320 mm and a thickness of 8 mm. Next, the heater electrode was placed on the molded body. The heater electrode is a Mo mesh (wire diameter 0.1 mm, mesh size #50, plain weave) cut into a predetermined pattern to match the resistance value of the heater electrode. Next, the granulated powder was further filled into the carbon mold and the heater electrode was embedded to fabricate a heater laminate. At this time, the granulated powder was filled and molded with a carbon punch so that the thickness from the upper surface of the heater electrode became 8 mm.

[0063] Next, plate-shaped Mo was placed on the heater laminate. Then, the granulated powder was further filled into the carbon mold on which Mo was placed to embed Mo. At this time, it was molded with a carbon punch so that the thickness became 8 mm from the upper surface of the plate-shaped Mo, and a laminate was produced. In this way, a heater laminate and a laminate in which a plate-shaped high melting point metal was laminated were produced.

[0064] Then, with the carbon punch inserted into the carbon mold, uniaxial hot press firing was performed at a temperature of 1800 °C, a pressure of 4 MPa, and in an N2 atmosphere for 4 hours. After firing, external shape processing (Φ300 mm × 18 mm) was performed. Drilling of terminal holes for connecting each electrode to an external power source, connection of terminals, and production of a necessary insulation structure were carried out simultaneously during the processing after firing. In this way, the electrode embedding member of Example 5 was produced.

[0065] (Evaluation) The produced heater module could be heated to 400 °C by energizing the heater electrode from an external power source.

[0066] Next, for the sample of Example 1, elemental analysis was performed on a cross-sectional cut surface perpendicular to the lamination direction by EPMA for mapping. Figures 5(a) to 5(d) are photographs showing the EPMA mapping of Example 1. Figure 5(a) is an SEM image of the analysis field of view of the cross section of Example 1. Figures 5(b) to 5(d) are photographs of mapping of Mo, Y, and O, respectively. The gray and white portions indicate the portions where Mo, Y, and O were detected, respectively.

[0067] As shown in Figures 5(a) to 5(d), it was found that Y and O are also present in the ceramic member (AlN), but are present more at the bonding interface between the ceramic member and the high melting point metal member (Mo). That is, it was confirmed that at the bonding interface between the ceramic member and the metal member, the concentration of the metal and the oxygen concentration that constitute the second phase of the ceramic member are respectively higher than the concentration of the metal and the oxygen concentration inside the ceramic member.

[0068] In the bonded body of the present invention, at the bonding interface between the ceramic member and the metal member, since metal and oxygen constituting the second phase of the ceramic member are present at high concentrations, it is highly likely that a chemical bond between Mo and AlN is formed through them. Further, in the manufacturing method of the present invention, since the recrystallization temperature of Mo is exceeded during sintering, Mo penetrates into the unevenness on the surface of the AlN sintered body due to plastic deformation of Mo at the bonding surface and exhibits an anchor effect, and it is presumed that even higher bonding strength can be obtained.

[0069] As described above, it was confirmed that the bonded body and the electrode-embedded member of the present invention can suppress erosion and contamination of the bonding surface, have strong bonding strength, and are bonded bodies and electrode-embedded members with a thick metal member. Further, it was confirmed that the manufacturing method of the present invention can manufacture such a bonded body or electrode-embedded member.

[0070] 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. Further, 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 Reference Numerals

[0071] 10 Bonded body 12 Laminate 20 Ceramic member 22 Granulated powder 30 Metal member 32 One main surface 34 The other main surface 36 Plate-shaped high melting point metal 40 Electrode 50 Electrode-embedded member 60 Carbon mold 70 Carbon punch

Claims

1. A joined body of a ceramic member mainly composed of AlN and a metal member made of Mo, W, or a Mo alloy as a refractory metal having a melting point of 2000 °C or higher, wherein the ceramic member has electrodes embedded therein, the ceramic member is joined to at least one main surface of the metal member, the ceramic member contains a second phase composed of Y₂O₃ as a metal oxide, the metal member has a maximum thickness in a direction perpendicular to one main surface of the metal member of 1 mm or more, and the joined interface of the ceramic member and the metal member is characterized in that the concentration of the metal and the oxygen concentration constituting the second phase of the ceramic member are each greater than the concentration of the metal and the oxygen concentration inside the ceramic member.

2. The ceramic member contains Ti as a Group 4 metal, and the metal member is characterized in that Ti as a Group 4 metal has diffused therein. The joined body according to Claim 1.

3. The metal member contains 1 wt% or less of a second metal oxide. The joined body according to Claim 1 or Claim 2.

4. A ceramic member is further joined to the other main surface on the side facing one main surface of the metal member. The joined body according to any one of Claims 1 to 3.

5. A method for manufacturing a joined body of a ceramic member mainly composed of AlN and a metal member made of Mo, W, or a Mo alloy as a refractory metal having a melting point of 2000 °C or higher, comprising the steps of granulating a powder obtained by adding a raw material powder of Y₂O₃ as a metal oxide to an AlN raw material powder to produce a granulated powder, laminating the granulated powder or a molded body formed from the granulated powder and the plate-shaped refractory metal having a thickness of 1 mm or more in a carbon mold such that one main surface of the plate-shaped refractory metal is perpendicular to the lamination direction, embedding electrodes in the molded body or laminating the electrodes in the carbon mold so as to sandwich the molded body, inserting a carbon punch into the carbon mold to form a laminate, and uniaxially pressure-sintering the laminate. A method for manufacturing a joined body, characterized by including these steps.

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