JP2023025496A - Joined body, method for manufacturing the same, and electrode embedding member - Google Patents

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 The present invention relates to a bonded body, a manufacturing method thereof, and an electrode-embedded member.

AlN members used in semiconductor manufacturing equipment are sometimes joined to metal members for the purpose of adding various functions.

Patent Literature 1 discloses a joined body and a semiconductor holding device in which an aluminum nitride member and a metal member are joined with Al brazing material. As a preferred embodiment, 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. An example is disclosed that is a member. It also discloses that the heat transfer member is made of tungsten, molybdenum, copper, or an alloy thereof. These metal members function as heat sinks and have a certain thickness.

In addition, in Patent Document 2, a sintered metal layer having a relatively large thickness and high conductivity is incorporated, and warping is suppressed to an extremely low level. A sintered metal layer made of tungsten or molybdenum and having a thickness of 15 to 100 μm is provided on at least a part of the bonding surface for the purpose of providing an aluminum nitride bonded body that has high strength and is suitable for use as an electrode-embedded member, and a method for manufacturing the same. is formed of aluminum nitride sintered bodies, wherein the sintered metal layer has a sheet resistance value of 1 Ω/□ or less and a warp of the sintered metal layer of 100 μm/100 mm or less A conjugate is disclosed.

JP-A-9-249465 JP-A-2005-159334 JP-A-5-246769 JP-A-62-78167

Journal of the Japan Institute of Metals, Vol. 45, No. 2 (1981) p. 184-P. 189

AlN ceramics used in semiconductor manufacturing processes are sometimes integrated with high-melting-point metals (metals with a melting point of 2000° C. or higher) used for heat sinks and the like. For this purpose, the refractory metal must have a certain thickness or more, but the sintered metal layer as disclosed in Patent Document 2 cannot have such a structure.

In addition, according to Non-Patent Document 1, it has been considered difficult to produce a bonded body because AlN and a high-melting-point metal do not react without a bonding material. Therefore, conventionally, a joined body of AlN ceramic and a high-melting-point metal has been manufactured by a method of joining by interposing a brazing material or the like at the joint interface (Patent Documents 1, 3, and 4).

However, when these bonded bodies are used in a semiconductor manufacturing process, the methods of Patent Documents 1, 3, and 4 raise concerns about erosion of the brazing material that is the bonding layer and contamination from the bonding layer. Therefore, an AlN-high melting point metal joined body, which is a joined body of AlN ceramic and a thick high melting point metal, and which suppresses the risk of contamination and corrosion from the joining material, has been desired.

SUMMARY OF THE INVENTION The present invention has been made in view of such circumstances, and a joined body in which erosion and contamination of the joint surface can be suppressed, joint strength is high, and the thickness of the metal member is large, a method for producing the same, and an electrode-embedded member intended to provide

(1) In order to achieve the above object, a joined body of the present invention is a joined body of a ceramic member containing AlN as a main component and a metal member made of a high melting point metal having a melting point of 2000° C. or higher, wherein the ceramic member is bonded to at least one main surface of the metal member, the ceramic member includes a second phase composed of a metal oxide, and the metal member has a maximum It has a thickness of 1 mm or more, and the bonding interface between the ceramic member and the metal member has a concentration of the metal and an oxygen concentration that constitute the second phase of the ceramic member, and a concentration of the metal inside the ceramic member and It is characterized by being larger than the oxygen concentration.

Thus, the metal concentration and oxygen concentration of the second phase at the bonding interface between the ceramic member containing AlN as a main component and the metal member made of a high-melting-point metal are higher than the metal concentration and oxygen concentration inside the ceramic member. Since each of them is large, the ceramic member and the metal member are joined via these, and a joined body in which erosion and contamination of the joining surfaces are suppressed can be obtained. In addition, since the thickness of the metal member is large, it can be used for various purposes such as using the metal member as a heat sink or 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 the maximum thickness is preferably 1 mm or more.

(2) In the joined body of the present invention, the ceramic member contains a Group 4 metal, and the metal member has the Group 4 metal diffused therein.

In this way, the ceramic member contains the Group 4 metal, and the Group 4 metal is diffused in the metal member, so that the bonding strength between the ceramic member and the metal member increases, and the reliability of the bonded body increases. get higher

(3) Further, in the joined body of the present invention, the metal member contains 1 wt % or less of the second metal oxide.

In this way, when the metal member contains 1 wt % or less of the second metal oxide, the bonding strength between the ceramic member and the metal member increases, and the reliability of the bonded body increases.

(4) In addition, the joined body of the present invention is characterized in that a ceramic member is further joined to the other main surface of the metal member facing the one main surface.

By joining the ceramic member to both main surfaces of the metal member in this way, the application of the joined body is further expanded.

(5) Further, an electrode-embedded member of the present invention is characterized by comprising the joined body according to any one of the above (1) to (3) and an electrode embedded in the ceramic member of the joined body. there is

Since AlN has a high thermal conductivity and a high insulating property, an electrode-embedded member in which an electrode is embedded in a ceramic member and a joint body of a ceramic member and a metal member can be used as a heater module with excellent thermal conductivity.

(6) Further, a method for manufacturing a bonded body of the present invention is a method for manufacturing a bonded body of a ceramic member containing AlN as a main component and a metal member made of a high melting point metal having a melting point of 2000° C. or higher, wherein the AlN raw material powder a step of granulating a powder obtained by adding a metal oxide raw material powder to a granulated powder to produce a granulated powder; the granulated powder or a molded body formed from the granulated powder; are stacked in a carbon mold so that one main surface of the plate-like high-melting-point metal is perpendicular to the stacking direction; inserting a carbon punch into the carbon mold to form a laminate; and a step of sintering the laminate under uniaxial pressure.

As a result, it is possible to obtain a joined body of the ceramic member and the metal member in which corrosion and contamination of the joining surfaces are suppressed. Since the thickness of the metal member is large, it can be used for various purposes such as using the metal member as a heat sink and increasing the strength and dimensional accuracy of the ceramic member.

According to the present invention, it is possible to obtain a joined body in which erosion and contamination of the joining surfaces of a ceramic member mainly composed of AlN and a metal member made of a high-melting-point metal are suppressed. In addition, since the thickness of the metal member is large, it can be used for various purposes such as using the metal member as a heat sink and increasing the strength and dimensional accuracy of the ceramic member.

1 is a schematic cross-sectional view showing an example of a joined body according to an embodiment of the present invention; FIG. FIG. 5 is a schematic cross-sectional view showing a modified example of the joined body according to the embodiment of the present invention; 1 is a schematic cross-sectional view showing an example of an electrode-embedded member according to an embodiment of the present invention; FIG. 4A to 4E are cross-sectional views schematically showing one stage of the manufacturing process of the manufacturing method according to the embodiment of the present invention, respectively; FIG. (a) is a cross-sectional SEM image of Example 1; (b) to (d) are photographs showing the mapping of EPMA analysis of the cross section of Example 1, respectively.

Next, embodiments of the present invention will be described with reference to the drawings. In order to facilitate understanding of the description, the same reference numerals are given to the same components in each drawing, and overlapping descriptions are omitted. In addition, in the configuration diagram, the size of each component is conceptually represented, and does not necessarily represent the actual size ratio.

[Embodiment]
[Structure of conjugate]
First, a bonded 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 invention. A bonded body 10 according to an embodiment of the present invention is formed by bonding a ceramic member 20 mainly composed of AlN and a metal member 30 made of a high-melting-point metal. A ceramic member containing AlN as a main component means containing 90 wt % or more of AlN. A metal member made of a high-melting-point metal can be molybdenum (Mo), tungsten (W), tantalum (Ta), or the like, which has a melting point of 2000° C. or higher, and refers to a material with a purity of 99 wt % or higher. As a result, deformation of the metal member 30 is suppressed even at the temperature during uniaxial pressure firing. 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 bonding interface between AlN and the metal member 30 can be suppressed. .

The joined body 10 has a ceramic member 20 joined to at least one main surface of a metal member 30 . Moreover, the metal member 30 preferably has a maximum diameter of 50% or more of the maximum diameter of the ceramic member 20 . Also, the ceramic member 20 is preferably bonded to the entire one main surface of the metal member 30 . By having these characteristics, the metal member 30 can be applied in a form suitable for various uses. Moreover, it is preferable that the ceramic member 20 is directly bonded to one main surface of the metal member 30 without interposing another member. This is because if another member is interposed, the bonding strength may decrease.

The ceramic member 20 contains a second phase of metal oxide. The metal constituting the metal oxide of the second phase is preferably one or more selected from Y and Ca, more preferably Y. The metal oxide that constitutes the second phase may be a sintering aid for a ceramic member containing AlN as a main component. In that case, the metal oxide constituting the second phase may be added in a necessary amount 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 Y ₂ O ₃ .

Metal member 30 has a maximum thickness of 1 mm or more in a direction perpendicular to one main surface 32 of metal member 30 . Since the metal member 30 is thick as described above, the metal member 30 can be used as a heat sink or a heat spreader, and can be applied to various applications such as 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 metal member 30 having a large thickness means that the maximum thickness of the metal member 30 in a direction perpendicular to one main surface 32 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 is not sufficiently exhibited, so the maximum thickness is preferably 1 mm or more.

It is preferable that the maximum thickness of the metal member 30 in the direction perpendicular to one main surface 32 is set according to the intended use. Considering that there was no metal member 30 joined with a large thickness like the present invention, the thickness is preferably 2 mm or more, more preferably 3 mm or more, and 4 mm or more depending on the application. is more preferred.

At the bonding interface between the ceramic member 20 and the metal member 30 , the metal concentration and oxygen concentration that constitute the second phase of the ceramic member 20 are higher than the metal concentration and oxygen concentration inside the ceramic member 20 . In this way, the metal concentration and oxygen concentration forming the second phase at the joint interface between the ceramic member 20 mainly composed of AlN and the metal member 30 made of a high-melting-point metal correspond to the metal concentration and oxygen concentration inside the ceramic member 20. Since the respective oxygen concentrations are higher than the oxygen concentration, the ceramic member 20 and the metal member 30 are joined via these, and a joined body in which erosion and contamination of the joint surfaces are suppressed is obtained.

Note that the bonding interface between the ceramic member 20 and the metal member 30 refers to an interface where the concentration of the metal element that mainly constitutes the metal member 30 sharply decreases in cross-sectional elemental mapping by EDX or EPMA. Further, the inside of the ceramic member 20 indicates a region which is at least 1 mm away from the bonding interface and where the concentration of the metal forming the second phase of the ceramic member 20 is uniform.

The change in concentration of the metal present in the ceramic member 20, the metal member 30, or the joint interface thereof can be performed by comparing the intensity (number of counts) of the characteristic X-rays of the relevant region by EPMA. This makes it possible to relatively evaluate the difference in metal and oxygen concentrations near and inside the interface.

Preferably, the ceramic member 20 further contains a Group 4 metal, and the metal member 30 has the Group 4 metal diffused therein. In this manner, the ceramic member 20 contains the Group 4 metal, and the Group 4 metal is diffused in the metal member 30, so that the bonding strength between the ceramic member 20 and the metal member 30 is increased, resulting in a bonded body. 10 becomes more reliable. The Group 4 metal is preferably one or more selected from Ti and Hf, more preferably Ti.

The metal member 30 preferably contains 1 wt % or less of the second metal oxide. When the metal member 30 contains 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 joined body 10 is increased. The metal constituting the second metal oxide is preferably one or more selected from Y, Ce, and Ca, and more preferably Y or Ce. The metal forming the second metal oxide may be the same as the metal forming the second phase metal oxide of the ceramic member 20 . These metal oxide components preliminarily contained in the metal member 30 increase the concentration of metal and oxygen at the bonding interface, thereby increasing the bonding strength.

FIG. 2 is a schematic cross-sectional view showing a modification of the joined body according to the embodiment of the invention. As shown in FIG. 2, it is preferable that the ceramic member 20 is further bonded to the main surface 34 of the metal member 30 on the side opposite to the main surface 32 . By bonding the ceramic member 20 to both main surfaces of the metal member 30 in this way, the application of the bonded body 10 is further expanded. Moreover, by sandwiching the plate-like high-melting-point metal (metal member 30) between the ceramic members 20, warping of the joined body 10 can be suppressed, and the joined body 10 with high dimensional accuracy can be manufactured. In addition, one principal surface 32 and the other principal surface 34 are collectively referred to as both principal surfaces 32 and 34 or principal surfaces 32 and 34 . Also, the bonded body 10 may have the ceramic member 20 bonded to surfaces other than the main surfaces 32 and 34 .

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

The bonded body 10 is the bonded body 10 described above. 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 and a foil shape. Also, various materials such as molybdenum and tungsten can be used. Electrode 40 can be used as a heater electrode.

The electrode embedded member 50 may be provided with terminal holes and terminals (not shown).

The joined body and the electrode-embedded member of the present invention are members in which erosion and contamination of the joining surfaces of the ceramic member mainly composed of AlN and the metal member made of a high-melting-point metal are suppressed. In addition, the joined body and the electrode-embedded member of the present invention have various uses, such as using the metal member as a heat sink or heat spreader, or increasing the strength and dimensional accuracy of the ceramic member, because the thickness of the metal member is large. can be applied to

[Method for producing joined body]
Next, a method for manufacturing the joined body 10 configured as described above will be described. 4A to 4E are cross-sectional views schematically showing one stage of the manufacturing process of the manufacturing method according to the embodiment of the present invention.

First, granulated powder 22 is produced by granulating a powder obtained by adding metal oxide raw material powder to AlN raw material powder. The AlN raw material powder preferably has a high purity, and the purity is preferably 96% or higher, more preferably 98% or higher. Also, the average particle diameter 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. For example, when Y ₂ O ₃ is used as the metal oxide raw powder, 0.1 wt % to 5 wt % of Y ₂ O ₃ is added to the AlN raw powder, and a binder such as PVA, a dispersant, and a solvent are added. is added to prepare a slurry, and the granulated powder 22 is granulated using a spray dryer or the like.

Next, a plate-shaped high-melting-point metal 36 having a thickness of 1 mm or more is prepared, and the granulated powder 22 or a compact formed from the granulated powder, and the plate-shaped high-melting-point metal 36 having a thickness of 1 mm or more are combined into a plate-shaped high melting point metal. The melting point metal 36 is stacked on a bottomed carbon mold 60 (mold) so that one main surface of the melting point metal 36 is perpendicular to the stacking direction.

As another example of stacking compacts, the obtained granulated powder 22 is used to produce one or more compacts. As a method for molding the molded body, for example, a known method such as uniaxial pressure molding or cold isostatic pressing (CIP) method may be used. The method for forming the molded body is not limited to pressure molding, and can be applied to, for example, green sheet lamination or cast molding.

In the case of producing the electrode-embedded member 50, when the granulated powder 22 is laminated, the granulated powder 22 is temporarily pressed, the electrode 40 is placed, and the granulated powder 22 is added and temporarily pressed, or the compact is formed. The electrode 40 is embedded in the portion that will become the ceramics member 20 after sintering by stacking the electrodes 40 and then stacking the compacts.

Next, a carbon punch 70 is inserted into the carbon mold 60 to form the laminate 12 . The laminated body 12 may be composed of two layers of a layer of granulated powder 22 or compact that will become the ceramic member 20 after sintering and a plate-shaped high melting point metal 36 that will become the metal member 30 after sintering. The refractory metal 36 may be three layers sandwiched between layers of the granulated powder 22 or compact. Moreover, the side surface in the stacking direction may have a portion where the plate-like high-melting-point metal 36 is exposed, or the plate-like high-melting-point metal 36 may be covered with the granulated powder 22 or the compact. FIG. 4 shows a case where a plate-like high-melting-point metal 36 is covered with granulated powder 22 to produce three layers.

Next, the laminated body 12 is uniaxially pressure-fired to produce the joined body 10 . The firing conditions are, for example, a temperature of 1700° C. or more and 2000° C. or less, a pressure of 1 MPa or more, and the firing can be performed by holding for 0.1 hour or more and 10 hours or less.

After firing, a step of processing into a predetermined shape may be provided. At this time, if the side surface of the plate-shaped high-melting-point metal 36 in the stacking direction is covered with a 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 has three layers sandwiched between layers of the ceramic member 20, processing may be performed to remove a part of the ceramic member 20 or one of the ceramic members 20 entirely. Further, a step of processing the shape of the plate-shaped high-melting-point metal 36 may be provided. At this time, the plate-shaped high melting point metal 36 is processed so that the maximum thickness in the direction perpendicular to one main surface 32 is not less than 1 mm.

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.

In addition, in the method of forming and laminating the molded body, a process of degreasing the molded body to produce a degreased body and a process of calcining the degreased body to produce a calcined 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, more preferably an air atmosphere. Further, for example, the calcination temperature is preferably 1200° C. or more and 1700° C. or less, and the calcination time is preferably 0.5 hours or more and 12 hours or less. The calcining atmosphere is preferably a nitrogen or inert gas atmosphere, but may be a vacuum atmosphere.

By such a method, it is possible to manufacture a joined body or an electrode-embedded member in which erosion and contamination of the joint surfaces of the ceramic member mainly composed of AlN and the metal member made of a high-melting-point metal are suppressed.

[Example]
(Preparation of conjugate)
(Example 1)
5 wt % of Y ₂ O ₃ was added to the AlN raw material powder, and a binder (PVA), dispersant and solvent were added to prepare a slurry, and a granulated powder was granulated with a spray dryer. In addition, Mo having a diameter of Φ50 mm and a thickness of 5 mm was prepared as a plate-shaped high-melting-point metal serving as a metal member.

Next, the granulated powder was filled in a carbon mold with a bottom and press-molded with a carbon punch to produce a compact having a diameter of 80 mm and a thickness of 10 mm. Next, Mo was placed on the compact. Next, the carbon mold was further filled with granulated powder to embed Mo. At this time, granulated powder was filled and molding was performed with a carbon punch so that the thickness from the upper surface of Mo was 10 mm.

Then, with the carbon punch inserted in the carbon mold, uniaxial hot press firing was performed at a temperature of 1800° C., a pressure of 4 MPa, and an N ₂ 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 of 3 mm×4 mm×19 mm were cut out so that the lamination direction was the long side.

(Example 2)
The bonded body of Example 2 was produced in the same process and under the same conditions, except that the granulated powder of Example 1 was changed to AlN raw material powder with 5 wt% Y ₂ O ₃ and 0.9 wt% TiN added. was made.

(Example 3)
A bonded body of Example 3 was produced in the same process and under the same conditions, except that the refractory metal of Example 1 was replaced with an alloy in which 0.4 wt % of Y ₂ O ₃ was added to Mo.

(Example 4)
A joined body of Example 4 was produced in the same process and under the same conditions except that the high-melting-point metal of Example 1 was replaced with W.

(Measurement of bonding strength)
The bonding strength of the bonded body was measured by a three-point bending strength test based on JIS R1601 2008 (testing method for room temperature bending strength of fine ceramics). The span was set to 10 mm, the joint surface was placed in the center in the longitudinal direction, and the knife edge was aligned with the joint surface for measurement. 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.

(Measurement result)
It was found that Example 1 had a bonding strength of 77 MPa and Example 4 had a bonding strength of 90 MPa, indicating that sufficient bonding strength was obtained. Example 2 had a bonding strength of 115 MPa, which was higher than that of the sample of Example 1. Moreover, Example 3 had a bonding strength of 103 MPa, which was higher than that of the sample of Example 1.

(Example 5)
(Preparation of electrode embedded member)
In Example 5, a heater electrode was embedded in the AlN sintered body (ceramic member) located on Mo in the manufacturing method of Example 1 to produce a heater module that can be used in a high-temperature process.

The same granulated powder as in Example 1 was prepared. Further, a plate-shaped Mo with a diameter of Φ300 mm and a thickness of 8 mm was prepared as a plate-shaped high-melting-point metal to be a metal member.

First, a heater laminate was produced. The granulated powder was filled in a bottomed carbon mold and press-molded with a carbon punch to prepare a compact having a diameter of Φ320 mm and a thickness of 8 mm. Next, a heater electrode was placed on the compact. The heater electrode is obtained by cutting Mo mesh (wire diameter 0.1 mm, mesh size #50, plain weave) into a predetermined pattern to match the resistance value of the heater electrode. Next, the carbon mold was further filled with the granulated powder, and the heater electrodes were embedded in the carbon mold to prepare a heater laminate. At this time, granulated powder was filled and a carbon punch was used to form the heater electrode so that the thickness was 8 mm from the upper surface of the heater electrode.

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

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 an N ₂ atmosphere for 4 hours. After firing, the outer shape was processed (Φ300 mm×18 mm). The drilling of terminal holes for connecting the respective electrodes to an external power source, the connection of the terminals, and the preparation of the necessary insulating structure were simultaneously carried out during processing after firing. Thus, an electrode-embedded member of Example 5 was produced.

(evaluation)
The fabricated heater module could be heated to 400° C. by energizing the heater electrodes from an external power source.

Next, with respect to the sample of Example 1, a cut surface perpendicular to the stacking direction was subjected to elemental analysis by EPMA and mapped. 5(a) to (d) are photographs showing EPMA mapping in Example 1, respectively. FIG. 5( a ) is a SEM image of a cross-sectional analysis field of Example 1. FIG. 5(b)-(d) are photographs mapping Mo, Y, and O, respectively. Gray and white portions indicate portions where Mo, Y, and O were detected, respectively.

As shown in FIGS. 5(a) to (d), Y and O are also present in the ceramic member (AlN), but are It turns out that there are many. That is, it was confirmed that the metal concentration and oxygen concentration of the second phase of the ceramic member were higher than the metal concentration and oxygen concentration inside the ceramic member at the joint interface between the ceramic member and the metal member.

In the joined body of the present invention, the metal and oxygen that constitute the second phase of the ceramic member are present at a high concentration at the joint interface between the ceramic member and the metal member, and chemical bonding between Mo and AlN occurs through these. It is highly likely that In addition, in the production method of the present invention, since the recrystallization temperature of Mo is exceeded during sintering, Mo penetrates into the unevenness of the surface of the AlN sintered body due to plastic deformation of Mo at the joint surface, and exerts an anchor effect. It is presumed that even higher bonding strength can be obtained with

From the above, it was confirmed that the joined body and the electrode-embedded member of the present invention can suppress the erosion and contamination of the joint surface, have a high joining strength, and have a thick metal member. Moreover, it was confirmed that the manufacturing method of the present invention can manufacture such a bonded body or an electrode-embedded member.

It goes without saying that the present invention is not limited to the above-described embodiments, but extends to various modifications and equivalents within the spirit and scope of the present invention. Also, the structure, shape, number, position, size, etc. of the constituent elements shown in each drawing are for convenience of explanation, and may be changed as appropriate.

REFERENCE SIGNS LIST 10 joined body 12 laminated body 20 ceramic member 22 granulated powder 30 metal member 32 one principal surface 34 the other principal surface 36 plate-like high melting point metal 40 electrode 50 electrode embedded member 60 carbon mold 70 carbon punch

Claims (6)

A joined body of a ceramic member containing AlN as a main component and a metal member made of a high melting point metal having a melting point of 2000° C. or higher,
The ceramic member is bonded to at least one main surface of the metal member,
The ceramic member includes a second phase made of a metal oxide,
The metal member has a maximum thickness of 1 mm or more in a direction perpendicular to one main surface of the metal member,
The bonding interface between the ceramic member and the metal member is characterized in that the concentration of the metal and the concentration of oxygen constituting the second phase of the ceramic member are higher than the concentration of the metal and the concentration of oxygen inside the ceramic member. zygote to be. The ceramic member contains a Group 4 metal,
2. The joined body according to claim 1, wherein said metal member has said Group 4 metal diffused therein. 3. The joined body according to claim 1, wherein the metal member contains 1 wt % or less of the second metal oxide. 4. The joined body according to claim 1, further comprising a ceramic member joined to the other main surface of the metal member facing the one main surface. a joined body according to any one of claims 1 to 3;
and an electrode embedded in the ceramic member of the joined body. A method for manufacturing a joined body of a ceramic member containing AlN as a main component and a metal member made of a high melting point metal having a melting point of 2000° C. or higher,
a step of granulating a powder obtained by adding a metal oxide raw material powder to an AlN raw material powder to produce a granulated powder;
The granulated powder or a molded body formed from the granulated powder, and the plate-shaped high-melting-point metal having a thickness of 1 mm or more are placed so that one main surface of the plate-shaped high-melting-point metal is perpendicular to the stacking direction. A step of laminating in a carbon mold;
inserting a carbon punch into the carbon mold to form a laminate;
and a step of sintering the laminate under uniaxial pressure.

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