JP7709872B2 - Joint, manufacturing method thereof, and electrode-embedded member - Google Patents
Joint, manufacturing method thereof, and electrode-embedded memberInfo
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- JP7709872B2 JP7709872B2 JP2021130779A JP2021130779A JP7709872B2 JP 7709872 B2 JP7709872 B2 JP 7709872B2 JP 2021130779 A JP2021130779 A JP 2021130779A JP 2021130779 A JP2021130779 A JP 2021130779A JP 7709872 B2 JP7709872 B2 JP 7709872B2
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Description
本発明は、接合体、その製造方法、および電極埋設部材に関する。 The present invention relates to a joint, a manufacturing method thereof, and an electrode-embedded member.
半導体製造装置に用いられるAlN製部材は、様々な機能を付加することを目的として、金属部材と接合させることがあった。 AlN components used in semiconductor manufacturing equipment are sometimes joined to metal components to add various functions.
特許文献1には、窒化アルミニウム部材と金属部材がAlロウ材で接合された接合体および半導体保持装置が開示されている。好適な態様として、窒化アルミニウム部材が、半導体ウエハーを設置するための設置面を備えた半導体保持部材であり、金属部材が、半導体保持部材と外部との間で熱量の伝達を行うための熱伝達部材である例が開示されている。また、熱伝達部材の例として、タングステン、モリブデン、銅、またはこれらの合金によって形成する、と開示されている。これらの金属部材はヒートシンクとして機能し一定の厚さを有している。 Patent Document 1 discloses a joint 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 a mounting surface for mounting a semiconductor wafer, and the metal member is a heat transfer member for transferring heat between the semiconductor holding member and the outside. In addition, examples of heat transfer members are disclosed that are made of tungsten, molybdenum, copper, or alloys of these. These metal members function as heat sinks and have a certain thickness.
また、特許文献2には、比較的大きな厚みを有し且つ導電性の高い焼結金属層を内蔵し、しかも、反りの発生が極めて小さく抑えられ、さらには焼結金属層と基板との接合強度も高く、電極埋設部材の用途に好適な窒化アルミニウム接合体及びその製造方法を提供することを目的として、接合面の少なくとも一部に、厚み15~100μmのタングステン又はモリブデンよりなる焼結金属層が形成された窒化アルミニウム焼結体の接合体であって、前記焼結金属層のシート抵抗値が1Ω/□以下であり、且つ前記焼結金属層の反りが100μm/100mm以下である窒化アルミニウム接合体が開示されている。 Patent Document 2 discloses an aluminum nitride sintered body having a sintered metal layer of 15 to 100 μm thickness made of tungsten or molybdenum formed on at least a portion of the joining surface, with the objective of providing an aluminum nitride sintered body and a manufacturing method thereof that incorporates a sintered metal layer that is relatively thick and highly conductive, has extremely little warping, and has a high bonding strength between the sintered metal layer and the substrate, and is suitable for use as an electrode-embedded member, and the sheet resistance of the sintered metal layer is 1 Ω/□ or less, and the warping of the sintered metal layer is 100 μm/100 mm or less.
半導体製造プロセスで使用されるAlNセラミックは、ヒートシンク等に利用される高融点金属(融点が2000℃以上の金属)と一体化される場合があった。そのためには高融点金属は一定以上の厚みが必要であるが、特許文献2のような焼結金属層ではそのような構造とすることはできなかった。 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 in heat sinks, etc. To do this, the high-melting-point metal needs to be thicker than a certain amount, but such a structure cannot be achieved with a sintered metal layer such as that described in Patent Document 2.
また、非特許文献1によると、AlNと高融点金属は接合材なしでは反応しないため接合体を作製することは困難であるとされてきた。そのため、従来はAlNセラミックと高融点金属の接合体は、接合界面にロウ材等を介在させて接合する(特許文献1、3、4)方法で製作されていた。 According to Non-Patent Document 1, it has been said that it is difficult to create a bonded body because AlN and high-melting-point metals do not react without a bonding material. For this reason, conventionally, bonds between AlN ceramic and high-melting-point metals have been produced by joining them with a brazing material or the like at the bonding interface (Patent Documents 1, 3, 4).
しかし、これらの接合体を半導体製造プロセスで使用する場合、特許文献1、3、4の方法では、接合層であるロウ材の浸食、接合層からのコンタミネーションが懸念された。そのため、AlNセラミックと厚みの厚い高融点金属の接合体であって、接合材からのコンタミネーションや浸食の恐れを抑制したAlN-高融点金属接合体が望まれていた。 However, when these bonded bodies are used in semiconductor manufacturing processes, the methods of Patent Documents 1, 3, and 4 raise concerns about erosion of the brazing material that forms the bonding layer and contamination from the bonding layer. For this reason, there has been a demand for an AlN-high melting point metal bonded body that is a bonded body of AlN ceramic and a thick high melting point metal and that reduces the risk of contamination and erosion from the bonding material.
本発明は、このような事情に鑑みてなされたものであり、接合面の浸食やコンタミネーションを抑制でき、接合強度が強く、金属部材の厚みが厚い接合体、その製造方法、および電極埋設部材を提供することを目的とする。 The present invention was made in consideration of these circumstances, and aims to provide a bonded body that can suppress erosion and contamination of the bonded surface, has strong bonding strength, and has a thick metal member, a manufacturing method thereof, and an electrode-embedded member.
(1)上記の目的を達成するため、本発明の接合体は、AlNを主成分とするセラミックス部材および融点が2000℃以上の高融点金属としてのMo、W又はMo合金からなる金属部材の接合体であって、前記セラミックス部材は、電極が埋設され、前記セラミックス部材は、少なくとも前記金属部材の一方の主面に接合され、前記セラミックス部材は、金属酸化物としてのY 2 O 3 からなる第2相を含み、前記金属部材は、前記金属部材の一方の主面に垂直な方向の最大厚みが1mm以上であり、前記セラミックス部材および前記金 属部材の接合界面は、前記前記セラミックス部材の前記第2相を構成する金属の濃度および酸素濃度が、前記セラミックス部材の内部の前記金属の濃度および酸素濃度よりそれぞれ大きいことを特徴としている。 (1) In order to achieve the above object, the present invention provides a joined body of a ceramic member mainly composed of AlN and a metal member composed of Mo, W or a Mo alloy as a high melting point metal having a melting point of 2000° C or more, wherein the ceramic member has an electrode embedded therein, the ceramic member is joined to at least one main surface of the metal member, the ceramic member includes a second phase composed of Y2O3 as 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, and the joint interface between the ceramic member and the metal member has a metal concentration and an oxygen concentration constituting the second phase of the ceramic member that are greater than the metal concentration and the oxygen concentration inside the ceramic member, respectively.
このように、AlNを主成分とするセラミックス部材および高融点金属からなる金属部材の接合界面の第2相を構成する金属の濃度および酸素濃度が、セラミックス部材の内部の金属の濃度および酸素濃度よりそれぞれ大きいことで、これらを介してセラミックス部材と金属部材とが接合され、接合面の浸食やコンタミネーションを抑制した接合体が得られる。また、金属部材の厚みが厚いことで、金属部材をヒートシンクやヒートスプレッダーとして利用したり、セラミックス部材の強度や寸法精度を高めたりするなど、様々な用途に適用できる。金属部材の最大厚みが1mmより小さくなると寸法精度を高める効果が十分に発揮されなくなるため1mm以上であることが好ましい。 In this way, the concentration of the metal and oxygen constituting the second phase at the bonding interface between the ceramic member mainly composed of AlN and the metal member made of a high melting point metal are greater than the metal concentration and oxygen concentration inside the ceramic member, respectively, and the ceramic member and the metal member are bonded via these, resulting in a bonded body that suppresses erosion and contamination of the bonding surface. In addition, the thick metal member allows the metal member to be used for various purposes, such as as a heat sink or heat spreader, or to increase 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 increasing dimensional accuracy will not be fully exerted, so it is preferable that the maximum thickness be 1 mm or more.
(2)また、本発明の接合体において、前記セラミックス部材は、第4族の金属を含み、前記金属部材は、前記第4族の金属が拡散していることを特徴としている。 (2) In the bonded body of the present invention, the ceramic member contains a Group 4 metal, and the metal member has the Group 4 metal diffused therein.
このように、セラミックス部材が第4族の金属を含み、金属部材に第4族の金属が拡散していることで、セラミックス部材と金属部材との接合強度が強くなり、接合体の信頼性が高くなる。 In this way, the ceramic member contains a Group 4 metal, and the Group 4 metal is diffused into the metal member, which increases the bond strength between the ceramic member and the metal member and increases the reliability of the bonded structure.
(3)また、本発明の接合体において、前記金属部材は、第2の金属酸化物を1wt%以下含むことを特徴としている。 (3) In the bonded body of the present invention, the metal member is characterized in that it contains 1 wt % or less of a second metal oxide.
このように、金属部材が第2の金属酸化物を1wt%以下含むことで、セラミックス部材と金属部材との接合強度が強くなり、接合体の信頼性が高くなる。 In this way, by the metal member containing 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 improved.
(4)また、本発明の接合体は、前記金属部材の一方の主面に対向する側の他方の主面に、さらにセラミックス部材が接合されていることを特徴としている。 (4) The bonded body of the present invention is also characterized in that a ceramic member is further bonded to the other main surface of the metal member opposite to the one main surface of the metal member.
このように、金属部材の両方の主面にセラミックス部材が接合されることにより、接合体の用途がさらに拡大する。 In this way, by joining ceramic members to both main surfaces of a metal member, the range of uses for the joint is further expanded.
(5)また、本発明の電極埋設部材は、上記(1)から(3)のいずれかに記載の接合体と、前記接合体のセラミックス部材に埋設された電極と、を備えることを特徴としている。 (5) The electrode-embedded member of the present invention is characterized by comprising a joint body according to any one of (1) to (3) above and an electrode embedded in the ceramic member of the joint body.
AlNは熱伝導率が高く絶縁性が高いため、セラミックス部材および金属部材の接合体のセラミックス部材に電極を埋設した電極埋設部材は、熱伝導性に優れたヒーターモジュールとして利用することができる。 Since AlN has high thermal conductivity and high insulation, an electrode-embedded member in which electrodes are embedded in the ceramic member of a joint of a ceramic member and a metal member can be used as a heater module with excellent thermal conductivity.
(6)また、本発明の接合体の製造方法は、AlNを主成分とするセラミックス部材および融点が2000℃以上の高融点金属としてのMo、W又はMo合金からなる金属部材の接合体の製造方法であって、AlN原料粉に金属酸化物としてのY
2
O
3
の原料粉を添加した粉末を造粒して造粒粉を作製する工程と、前記造粒粉または前記造粒粉から形成した成形体、および厚み1mm以上の板状の高融点金属を、前記板状の高融点金属の一方の主面が積層方向に垂直になるようにカーボン型に積層する工程と、前記カーボン型にカーボンパンチを挿入し、積層体を形成する工程と、前記成形体に電極を埋設する、又は、前記電極を前記成形体で挟むように前記カーボン型に積層する工程と、前記積層体を一軸加圧焼成する工程と、を含むことを特徴としている。
(6) Also, the present invention provides a method for producing a joined body of a ceramic member mainly composed of AlN and a metal member composed of Mo, W or a Mo alloy as a high-melting point metal having a melting point of 2000°C or more, the method 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; stacking the granulated powder or a molded body formed from the granulated powder, and a plate-shaped high-melting point metal having a thickness of 1 mm or more on a carbon mold so that one main surface of the plate-shaped high-melting point metal is perpendicular to a stacking direction; inserting a carbon punch into the carbon mold to form a stack; embedding an electrode in the molded body, or stacking the electrode on the carbon mold so that the electrode is sandwiched between the molded bodies; and uniaxially pressing and sintering the stack.
これにより、接合面の浸食やコンタミネーションを抑制したセラミックス部材および金属部材の接合体が得られる。金属部材の厚みが厚いことで、金属部材をヒートシンクとして利用したり、セラミックス部材の強度や寸法精度を高めたりするなど、様々な用途に適用できる。 This results in a bonded ceramic and metal member that suppresses erosion and contamination of the bonding surfaces. The thick metal member can be used for a variety of purposes, such as using it as a heat sink or to increase the strength and dimensional accuracy of the ceramic member.
本発明によれば、AlNを主成分とするセラミックス部材および高融点金属からなる金属部材の接合面の浸食やコンタミネーションを抑制した接合体が得られる。また、金属部材の厚みが厚いことで、金属部材をヒートシンクとして利用したり、セラミックス部材の強度や寸法精度を高めたりするなど、様々な用途に適用できる。 According to the present invention, a bonded body is obtained in which erosion and contamination of the bonding surface between a ceramic member mainly composed of AlN and a metal member made of a high melting point metal is suppressed. In addition, since the metal member is thick, it can be used for various purposes, such as using the metal member as a heat sink or increasing the strength and dimensional accuracy of the ceramic member.
次に、本発明の実施の形態について、図面を参照しながら説明する。説明の理解を容易にするため、各図面において同一の構成要素に対しては同一の参照番号を付し、重複する説明は省略する。なお、構成図において、各構成要素の大きさは概念的に表したものであり、必ずしも実際の寸法比率を表すものではない。 Next, an embodiment of the present invention will be described with reference to the drawings. To facilitate understanding of the description, the same reference numbers are used for the same components in each drawing, and duplicate descriptions will be omitted. Note that in the configuration diagrams, the size of each component is shown conceptually and does not necessarily represent the actual dimensional ratio.
[実施形態]
[接合体の構成]
まず、本発明の実施形態に係る接合体を説明する。図1は、本発明の実施形態に係る接合体の一例を示す模式的な断面図である。本発明の実施形態に係る接合体10は、AlNを主成分とするセラミックス部材20および高融点金属からなる金属部材30が接合されて形成されている。AlNを主成分とするセラミックス部材とは、AlNを90wt%以上含むことをいう。また、高融点金属からなる金属部材とは、融点が2000℃以上のモリブデン(Mo)やタングステン(W)、タンタル(Ta)等が適用でき、純度99wt%以上のものを指す。これにより、一軸加圧焼成時の温度であっても金属部材30の変形が抑制される。また、同時にAlNと金属部材30との界面で900℃以上の比較的高温の融点を持つ高融点金属酸化物が形成されるため、AlNと金属部材30の接合界面の変形を抑制することができる。
[Embodiment]
[Configuration of the joint]
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 bonded body according to an embodiment of the present 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 mainly composed of AlN means that it contains 90 wt% or more of AlN. In addition, a metal member made of a high-melting point metal refers to one that can be applied with a melting point of 2000° C. or more, such as molybdenum (Mo), tungsten (W), tantalum (Ta), etc., and has a purity of 99 wt% or more. This suppresses deformation of the metal member 30 even at the temperature during uniaxial pressure firing. At the same time, a high-melting point metal oxide having a relatively high melting point of 900° C. or more is formed at the interface between AlN and the metal member 30, so that deformation of the bonding interface between AlN and the metal member 30 can be suppressed.
接合体10は、セラミックス部材20が少なくとも金属部材30の一方の主面に接合されている。また、金属部材30は、セラミックス部材20の最大径の50%以上の最大径を有することが好ましい。また、セラミックス部材20は、金属部材30の一方の主面の全面に接合されることが好ましい。これらの特徴を有することで、金属部材30を様々な用途に応じた形態で適用できる。また、セラミックス部材20は、金属部材30の一方の主面に他の部材を介さず直接接合されることが好ましい。他の部材を介すと、接合強度が小さくなる虞があるためである。 In the bonded body 10, the ceramic member 20 is bonded to at least one of the main surfaces of the metal member 30. The metal member 30 preferably has a maximum diameter that is 50% or more of the maximum diameter of the ceramic member 20. The ceramic member 20 is preferably bonded to the entire surface of one of the main surfaces of the metal member 30. These characteristics allow the metal member 30 to be used in a variety of forms according to various applications. The ceramic member 20 is preferably bonded directly to one of the main surfaces of the metal member 30 without using another member. This is because using another member may reduce the bond strength.
セラミックス部材20は、金属酸化物からなる第2相を含む。第2相の金属酸化物を構成する金属は、Y、Caから選択された1種類以上であることが好ましく、Yであることがより好ましい。第2相を構成する金属酸化物は、AlNを主成分とするセラミックス部材の焼結助剤であってもよい。その場合、第2相を構成する金属酸化物は、セラミックス部材の焼結助剤として必要な量添加されていてもよい。例えば、Yを焼結助剤として添加される場合、Y2O3換算で0.1wt%以上5wt%以下添加されてもよい。 The ceramic member 20 includes a second phase made of a metal oxide. The metal constituting the metal oxide of the second phase is preferably one or more selected from Y and Ca, and more preferably Y. The metal oxide constituting the second phase may be a sintering aid for a ceramic member mainly composed of AlN. 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 Y2O3 .
金属部材30は、金属部材30の一方の主面32に垂直な方向の最大厚みが1mm以上である。このように、金属部材30の厚みが厚いことで、金属部材30をヒートシンクやヒートスプレッダーとして利用したり、セラミックス部材20の強度や寸法精度を高めたりするなど、様々な用途に適用できる。金属部材30の一方の主面32とは、セラミックス部材20との接合面である。金属部材30の厚みが厚いとは、金属部材30の一方の主面32に垂直な方向の最大厚みが1mm以上であることとする。金属部材30の最大厚みが1mmより小さくなると寸法精度を高める効果が十分に発揮されなくなるため1mm以上であることが好ましい。 The metal member 30 has a maximum thickness of 1 mm or more in a direction perpendicular to one of the main surfaces 32 of the metal member 30. In this way, the metal member 30 has a large thickness, and can be used for various purposes, such as using the metal member 30 as a heat sink or heat spreader, or improving the strength and dimensional accuracy of the ceramic member 20. The one of the main surfaces 32 of the metal member 30 is the bonding surface with the ceramic member 20. The metal member 30 being thick means that the maximum thickness in a direction perpendicular to one of the main surfaces 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 is not fully exerted, so it is preferable that the thickness is 1 mm or more.
金属部材30の一方の主面32に垂直な方向の最大厚みは、適用する用途に応じた厚みにすることが好ましい。本発明のような金属部材30の厚みの厚い接合体がなかったことを考慮すると、用途によっては、例えば、2mm以上であることが好ましく、3mm以上であることがより好ましく、4mm以上であることがさらに好ましい。 The maximum thickness in the direction perpendicular to one of the main surfaces 32 of the metal member 30 is preferably set according to the intended application. Considering that there have been no joints with thick metal members 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.
セラミックス部材20および金属部材30の接合界面は、セラミックス部材20の第2相を構成する金属の濃度および酸素濃度が、セラミックス部材20の内部の当該金属の濃度および酸素濃度よりそれぞれ大きい。このように、AlNを主成分とするセラミックス部材20および高融点金属からなる金属部材30の接合界面の第2相を構成する金属の濃度および酸素濃度が、セラミックス部材20の内部の金属の濃度および酸素濃度よりそれぞれ大きいことで、これらを介してセラミックス部材20と金属部材30とが接合され、接合面の浸食やコンタミネーションを抑制した接合体が得られる。 At the bonding interface between the ceramic member 20 and the metal member 30, the concentration of the metal constituting the second phase of the ceramic member 20 and the oxygen concentration are greater than the concentration of the metal and the oxygen concentration inside the ceramic member 20, respectively. In this way, the concentration of the metal and the oxygen concentration of the second phase constituting 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 greater than the concentration of the metal and the oxygen concentration inside the ceramic member 20, respectively, so that the ceramic member 20 and the metal member 30 are bonded via these, and a bonded body in which erosion and contamination of the bonding surface is suppressed is obtained.
なお、セラミックス部材20および金属部材30の接合界面とは、EDXまたはEPMAによる断面の元素マッピングにおいて金属部材30を主に構成する金属元素が急激にその濃度を低下させる界面を指す。また、セラミックス部材20の内部とは、接合界面から少なくとも1mm離間しセラミックス部材20の第2相を構成する金属の濃度が一様である領域を示す。 The bonded interface between the ceramic member 20 and the metal member 30 refers to the interface where the concentration of the metal element that mainly constitutes the metal member 30 drops sharply in cross-sectional elemental mapping by EDX or EPMA. The inside of the ceramic member 20 refers to a region at least 1 mm away from the bonded interface where the concentration of the metal that constitutes the second phase of the ceramic member 20 is uniform.
セラミックス部材20、金属部材30、またはその接合界面に存在する金属の濃度変化は、EPMAによる当該領域の特性X線の強度(カウント数)の比較によって行うことができる。これにより界面近傍および内部の金属及び酸素濃度の差を相対的に評価することができる。 Changes in the concentration of metals present in the ceramic member 20, the metal member 30, or their joint interface can be determined by comparing the intensity (number of counts) of characteristic X-rays in the relevant area using EPMA. This allows for a relative evaluation of the differences in metal and oxygen concentration near and inside the interface.
セラミックス部材20は、さらに第4族の金属を含み、金属部材30は、当該第4族の金属が拡散していることが好ましい。このように、セラミックス部材20が第4族の金属を含み、金属部材30に第4族の金属が拡散していることで、セラミックス部材20と金属部材30との接合強度が強くなり、接合体10の信頼性が高くなる。第4族の金属は、Ti、Hfから選択された1種類以上であることが好ましく、Tiであることがより好ましい。 It is preferable that the ceramic member 20 further contains a Group 4 metal, and that the metal member 30 has the Group 4 metal diffused therein. In this way, the ceramic member 20 contains a Group 4 metal, and the metal member 30 has the Group 4 metal diffused therein, thereby increasing the bonding strength between the ceramic member 20 and the metal member 30, and increasing the reliability of the bonded body 10. It is preferable that the Group 4 metal is one or more selected from Ti and Hf, and more preferably Ti.
金属部材30は、第2の金属酸化物を1wt%以下含むことが好ましい。金属部材30が第2の金属酸化物を1wt%以下含むことで、セラミックス部材20と金属部材30との接合強度が強くなり、接合体10の信頼性が高くなる。第2の金属酸化物を構成する金属は、Y、Ce、Caから選択された1種類以上であることが好ましく、Y、またはCeであることがより好ましい。第2の金属酸化物を構成する金属は、セラミックス部材20の第2相の金属酸化物を構成する金属と同じであってもよい。金属部材30に予め含まれるこれらの金属酸化物成分が接合界面の金属や酸素濃度を高め、接合強度を高くすることができる。 It is preferable that the metal member 30 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 bonded body 10 is improved. The metal constituting the second metal oxide is preferably one or more selected from Y, Ce, and Ca, and is more preferably Y or Ce. The metal constituting the second metal oxide may be the same as the metal constituting the second phase metal oxide of the ceramic member 20. These metal oxide components already contained in the metal member 30 can increase the metal and oxygen concentration at the bonding interface, thereby increasing the bonding strength.
図2は、本発明の実施形態に係る接合体の変形例を示す模式的な断面図である。図2に示されるように、金属部材30の一方の主面32に対向する側の他方の主面34に、さらにセラミックス部材20が接合されていることが好ましい。このように、金属部材30の両方の主面にセラミックス部材20が接合されることにより、接合体10の用途がさらに拡大する。また、セラミックス部材20で板状の高融点金属(金属部材30)を挟み込むことにより、接合体10の反りを抑制することができ、寸法精度の高い接合体10を作製することができる。なお、一方の主面32および他方の主面34を合わせて、両方の主面32、34、または主面32、34という。また、接合体10は、主面32、34以外の面にセラミックス部材20が接合されていてもよい。 2 is a schematic cross-sectional view showing a modified example of the bonded body according to the embodiment of the present invention. As shown in FIG. 2, it is preferable that a ceramic member 20 is further bonded to the other main surface 34 of the metal member 30 opposite to the one main surface 32. In this way, by bonding the ceramic members 20 to both main surfaces of the metal member 30, the uses of the bonded body 10 are further expanded. In addition, by sandwiching a plate-shaped high-melting point metal (metal member 30) between the ceramic members 20, it is possible to suppress warping of the bonded body 10, and it is possible to produce a bonded body 10 with high dimensional accuracy. Note that the one main surface 32 and the other main surface 34 are referred to as both main surfaces 32, 34, or the main surfaces 32, 34 together. In addition, the bonded body 10 may have a ceramic member 20 bonded to a surface other than the main surfaces 32, 34.
[電極埋設部材の構成]
次に、本発明の実施形態に係る電極埋設部材を説明する。図3は、本発明の実施形態に係る電極埋設部材の一例を示す模式的な断面図である。本発明の実施形態に係る電極埋設部材50は、接合体10と、接合体10のセラミックス部材20に埋設された電極40と、を備える。
[Configuration 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 present invention. An electrode-embedded member 50 according to an embodiment of the present invention includes a bonded body 10 and an electrode 40 embedded in a ceramic member 20 of the bonded body 10.
接合体10は、上述した接合体10である。電極40は、接合体10のセラミックス部材20に埋設される。電極40の形状は、メッシュ状や箔状など、様々な形状とすることができる。また、材質も、モリブデン、タングステンなど、様々な材質とすることができる。電極40は、ヒーター用電極として使用できる。 The joined body 10 is the joined body 10 described above. The electrode 40 is embedded in the ceramic member 20 of the joined body 10. The electrode 40 can be in various shapes, such as a mesh shape or a foil shape. The electrode 40 can also be made of various materials, such as molybdenum and tungsten. The electrode 40 can be used as a heater electrode.
電極埋設部材50は、図示しない端子穴、端子が設けられていてもよい。 The electrode embedding member 50 may be provided with terminal holes and terminals (not shown).
本発明の接合体および電極埋設部材は、AlNを主成分とするセラミックス部材および高融点金属からなる金属部材の接合面の浸食やコンタミネーションを抑制した部材である。また、本発明の接合体および電極埋設部材は、金属部材の厚みが厚いことで、金属部材をヒートシンクやヒートスプレッダーとして利用したり、セラミックス部材の強度や寸法精度を高めたりするなど、様々な用途に適用できる。 The bonded body and electrode-embedded member of the present invention are members that suppress erosion and contamination of the bonding surface of a ceramic member whose main component is AlN and a metal member made of a high-melting point metal. In addition, since the thickness of the metal member of the bonded body and electrode-embedded member of the present invention is thick, the metal member can be used as a heat sink or heat spreader, or to increase the strength and dimensional accuracy of the ceramic member, making it applicable to a variety of uses.
[接合体の製造方法]
次に、上記のように構成された接合体10の製造方法を説明する。図4(a)~(e)は、それぞれ本発明の実施形態に係る製造方法の製造工程の一段階を模式的に示す断面図である。
[Method of manufacturing the bonded body]
Next, a method for manufacturing the bonded body 10 configured as described above will be described. Figures 4(a) to 4(e) are cross-sectional views each showing a schematic diagram of one stage of the manufacturing process of the manufacturing method according to the embodiment of the present invention.
まず、AlN原料粉に金属酸化物原料粉を添加した粉末を造粒して造粒粉22を作製する。AlN原料粉末は、高純度であることが好ましく、その純度は、好ましくは96%以上、より好ましくは98%以上である。また、AlN粉末の平均粒径は、好ましくは0.1μm以上1.0μm以下、より好ましくは0.3μm以上0.8μm以下である。金属酸化物原料粉として、例えばY2O3を用いる場合は、AlN原料粉に内比で0.1wt%~5wt%のY2O3を添加し、PVA系等のバインダ、分散剤、溶剤を添加してスラリーを調製し、スプレードライヤー等により造粒粉22を造粒する。 First, the metal oxide raw powder is added to the AlN raw powder, and the resulting powder is granulated to produce the granulated powder 22. The AlN raw powder is preferably highly pure, and the purity is preferably 96% or more, more preferably 98% or more. 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 Y 2 O 3 is used as the metal oxide raw powder, for example, 0.1 wt % to 5 wt % of Y 2 O 3 is added to the AlN raw powder, 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.
次に、厚み1mm以上の板状の高融点金属36を準備し、造粒粉22または造粒粉から形成した成形体、および厚み1mm以上の板状の高融点金属36を、板状の高融点金属36の一方の主面が積層方向に垂直になるように有底のカーボン型60(成形型)に積層する。 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 stacked in a bottomed carbon mold 60 (molding mold) so that one main surface of the plate-shaped high melting point metal 36 is perpendicular to the stacking direction.
成形体を積層する他の例として、得られた造粒粉22を用いて1または複数の成形体を作製する。成形体の成形方法としては、例えば、一軸加圧成形や冷間静水等方圧加圧(CIP:Cold Isostatic Pressing)法などの公知の方法を用いればよい。なお、成形体を形成する方法は、加圧成形に限らず、例えば、グリーンシート積層、または鋳込み成形であっても適用が可能である。 As another example of stacking the green bodies, one or more green bodies are produced using the obtained granulated powder 22. The green bodies can be formed by known methods such as uniaxial pressing or cold isostatic pressing (CIP). The method of forming the green bodies is not limited to pressing, and can also be, for example, green sheet stacking or casting.
電極埋設部材50を作製する場合は、造粒粉22を積層する際に、造粒粉22を仮プレスし電極40を配置しさらに造粒粉22を投入し仮プレスする、または、成形体を積層し電極40を配置しさらに成形体を積層することで、焼結後セラミックス部材20となる部分に電極40が埋設される。 When producing the electrode-embedded member 50, the granulated powder 22 is temporarily pressed when it is stacked, the electrode 40 is placed, and the granulated powder 22 is further added and temporarily pressed, or the compacts are stacked, the electrode 40 is placed, and the compacts are further stacked, so that the electrode 40 is embedded in the portion that will become the ceramic member 20 after sintering.
次に、カーボン型60にカーボンパンチ70を挿入し、積層体12を形成する。積層体12は、焼結後セラミックス部材20となる造粒粉22または成形体の層と、焼結後金属部材30となる板状の高融点金属36の2層であってもよいし、板状の高融点金属36が造粒粉22または成形体の層で挟まれた3層であってもよい。また、積層方向の側面は、板状の高融点金属36が露出する部分があってもよいし、板状の高融点金属36が造粒粉22または成形体で覆われていてもよい。図4は、板状の高融点金属36が造粒粉22で覆われて、3層で作製される場合を示している。 Next, a carbon punch 70 is inserted into the carbon mold 60 to form the laminate 12. The laminate 12 may be two layers, a layer of granulated powder 22 or a molded body 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, or it may be three layers in which the plate-shaped high-melting point metal 36 is sandwiched between layers of granulated powder 22 or a molded body. In addition, the side surface in the stacking direction may have 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 molded body. Figure 4 shows a case where the plate-shaped high-melting point metal 36 is covered with the granulated powder 22 and is made into three layers.
次に、積層体12を一軸加圧焼成することで接合体10を作製する。焼成条件は、例えば、1700℃以上2000℃以下の温度、1MPa以上の圧力で、0.1時間以上10時間以下保持することで焼成することができる。 Next, the laminate 12 is uniaxially pressurized and sintered to produce the bonded body 10. The sintering conditions are, for example, a temperature of 1700°C to 2000°C, a pressure of 1 MPa or more, and a holding time of 0.1 hours to 10 hours.
焼成後、所定の形状に加工する工程を設けてもよい。このとき、板状の高融点金属36の積層方向の側面がセラミックス部材で覆われている場合、板状の高融点金属36を露出する加工を行なってもよい。また、板状の高融点金属36がセラミックス部材20の層で挟まれた3層である場合、セラミックス部材20のうちの一部、または一方のセラミックス部材20を全部取り去る加工をしてもよい。また、板状の高融点金属36の形状を加工する工程を設けてもよい。このときは、板状の高融点金属36の一方の主面32に垂直な方向の最大厚みが1mmを下回らないように加工をする。 After firing, a process may be provided to process the plate-shaped high-melting point metal 36 into a predetermined shape. At this time, if the side surface in the stacking direction of the plate-shaped high-melting point metal 36 is covered with a ceramic member, processing may be performed to expose the plate-shaped high-melting point metal 36. Also, if the plate-shaped high-melting point metal 36 is a three-layer structure sandwiched between layers of ceramic members 20, processing may be performed to remove a part of the ceramic members 20 or all of one of the ceramic members 20. Also, a process may be provided to process the shape of the plate-shaped high-melting point metal 36. At this time, processing is performed so that the maximum thickness of the plate-shaped high-melting point metal 36 in the direction perpendicular to one main surface 32 does not fall below 1 mm.
また、電極埋設部材50とした場合は、電極40の一部を露出させる工程や、電極40に端子を接続する工程を設けてもよい。 In addition, when an electrode-embedded member 50 is used, a process for exposing a portion of the electrode 40 and a process for connecting a terminal to the electrode 40 may be provided.
なお、成形体を作製し積層する方法では、成形体を脱脂して脱脂体を作製する工程や脱脂体を仮焼して仮焼体を作製する工程を設けてもよい。その場合、例えば、脱脂温度は400℃以上800℃以下であることが好ましく、脱脂時間は1時間以上120時間以下であることが好ましい。脱脂雰囲気は、大気雰囲気または窒素雰囲気であることが好ましく、大気雰囲気であることがより好ましい。また、例えば、仮焼温度は1200℃以上1700℃以下であることが好ましく、仮焼時間は、0.5時間以上12時間以下であることが好ましい。仮焼雰囲気は、窒素や不活性ガス雰囲気であることが好ましいが、真空などの雰囲気であってもよい。 In addition, the method of producing and laminating a molded body may include a step of degreasing the molded body to produce a degreased body and a step of calcining the degreased body to produce a calcined body. In this 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 higher and 120 hours or lower. The degreasing atmosphere is preferably an air atmosphere or a nitrogen atmosphere, and more preferably an air atmosphere. Also, for example, the calcination temperature is preferably 1200°C or higher and 1700°C or lower, and the calcination time is preferably 0.5 hours or higher and 12 hours or lower. The calcination atmosphere is preferably a nitrogen or inert gas atmosphere, but may be a vacuum atmosphere or the like.
このような方法により、AlNを主成分とするセラミックス部材および高融点金属からなる金属部材の接合面の浸食やコンタミネーションを抑制した接合体または電極埋設部材を製造することができる。 This method makes it possible to manufacture a joint or electrode-embedded member that suppresses erosion and contamination of the joint surface between a ceramic member whose main component is AlN and a metal member made of a high-melting point metal.
[実施例]
(接合体の作製)
(実施例1)
AlN原料粉に内比で5wt%のY2O3を添加し、バインダ(PVA)、分散剤、溶剤を添加してスラリーを調製し、スプレードライヤーにより造粒粉を造粒した。また、金属部材となる板状の高融点金属として、径Φ50mm、厚み5mmのMoを準備した。
[Example]
(Preparation of Conjugate)
Example 1
5 wt % of Y2O3 was added to the AlN raw material powder, and a binder (PVA), a dispersant, and a solvent were added to prepare a slurry, which was then granulated by a spray dryer.Mo with a diameter of Φ50 mm and a thickness of 5 mm was prepared as a plate-shaped high-melting point metal to be the metal member.
次に、造粒粉を有底のカーボン型に充填し、カーボンパンチでプレス成形し、径Φ80mm、厚み10mmの成形体を作製した。次に、Moを成形体上に載置した。次に、カーボン型に造粒粉をさらに充填してMoを埋設した。このとき、Moの上面より厚みが10mmになるように、造粒粉の充填およびカーボンパンチでの成形をした。 Next, the granulated powder was filled into a bottomed carbon mold and pressed 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 carbon mold was further filled with granulated powder to embed the Mo. At this time, the granulated powder was filled and molded with the carbon punch so that the thickness from the top surface of the Mo was 10 mm.
そして、カーボンパンチをカーボン型に挿入した状態で、温度1800℃、圧力4MPa、N2雰囲気で2時間一軸ホットプレス焼成を行った。これにより直径80mmのAlN焼結体の内部に直径50mmのMoからなる金属部材を埋設することができた。このようにして、実施例1の接合体を作製した。その後、積層方向が長辺となるように3mm×4mm×19mmの実施例1の試験片を複数切り出した。 Then, with the carbon punch inserted into the carbon mold, uniaxial hot press sintering was performed for 2 hours at a temperature of 1800°C, a pressure of 4 MPa, and a N2 atmosphere. As a result, a metal member made of Mo with a diameter of 50 mm could be embedded inside an AlN sintered body with a diameter of 80 mm. In this way, the bonded body of Example 1 was produced. After that, multiple test pieces of Example 1 with dimensions of 3 mm x 4 mm x 19 mm were cut out so that the lamination direction was the long side.
(実施例2)
実施例1の造粒粉を、AlN原料粉に内比で5wt%のY2O3および0.9wt%のTiNを添加したものに変更した以外、同じ工程、条件で実施例2の接合体を作製した。
Example 2
A joint body of Example 2 was produced under the same process and conditions as Example 1, except that the granulated powder of Example 1 was changed to AlN raw material powder to which 5 wt % of Y 2 O 3 and 0.9 wt % of TiN were added.
(実施例3)
実施例1の高融点金属を、MoにY2O3が0.4wt%添加された合金に置き換えた以外、同じ工程、条件で実施例3の接合体を作製した。
Example 3
A joint body of Example 3 was produced under the same process and conditions as Example 1, except that the high melting point metal was replaced with an alloy of Mo with 0.4 wt % Y 2 O 3 added.
(実施例4)
実施例1の高融点金属を、Wに置き換えた以外、同じ工程、条件で実施例4の接合体を作製した。
Example 4
A joint body of Example 4 was produced using the same process and conditions as in Example 1, except that the high melting point metal was replaced with W.
(接合強度の測定)
JIS R1601 2008(ファインセラミックスの室温曲げ強さ試験方法)に準拠した3点曲げ強度試験により、接合体の接合強度の測定を行なった。スパンは10mmとし、長手方向の中央部に接合面を配置してナイフエッジを接合面に合わせて測定を行なった。試験片は各試料5個準備し、5個の測定値の平均値を各試料の接合強度の値とした。
(Measurement of Bonding Strength)
The bond strength of the bonded bodies was measured by a three-point bending strength test in accordance with JIS R1601 2008 (room temperature bending strength test method for fine ceramics). The span was 10 mm, and the bond surface was placed at the center in the longitudinal direction, and the measurement was performed by aligning the knife edge with the bond surface. Five test pieces were prepared for each sample, and the average of the five measurements was used as the bond strength value for each sample.
(測定結果)
実施例1は、接合強度が77MPa、実施例4は90MPaとなり、十分な接合強度が得られていることが分かった。実施例2は、接合強度が115MPaとなり、実施例1の試料より高い接合強度が得られた。また、実施例3は、103MPaとなり、実施例1の試料より高い接合強度が得られた。
(Measurement results)
It was found that sufficient bonding strength was obtained, with the bonding strength being 77 MPa in Example 1 and 90 MPa in Example 4. The bonding strength was 115 MPa in Example 2, which was higher than that of the sample in Example 1. Moreover, the bonding strength was 103 MPa in Example 3, which was higher than that of the sample in Example 1.
(実施例5)
(電極埋設部材の作製)
実施例5は、実施例1の製法においてMoの上に位置するAlN焼結体(セラミックス部材)にヒーター電極を埋設し、高温下のプロセスで使用できるヒーターモジュールを作製した。
Example 5
(Preparation of electrode-embedded member)
In Example 5, a heater electrode was embedded in an AlN sintered body (ceramic member) located on Mo in the manufacturing method of Example 1, to fabricate a heater module that can be used in processes under high temperatures.
造粒粉は、実施例1と同様のものを準備した。また、金属部材となる板状の高融点金属として、径Φ300mm、厚み8mmの板状のMoを準備した。 The granulated powder was prepared in the same manner as in Example 1. In addition, 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 used as the metal member.
まず、ヒーター積層体を作製した。造粒粉を有底のカーボン型に充填し、カーボンパンチでプレス成形し、径Φ320mm厚み8mmの成形体を作製した。次に、ヒーター電極を成形体上に載置した。ヒーター電極はMoメッシュ(線径0.1mm、メッシュサイズ#50、平織)をヒーター電極の抵抗値を合わせるため所定のパターンに裁断したものである。次に、カーボン型に造粒粉をさらに充填してヒーター電極を埋設することでヒーター積層体を作製した。このとき、ヒーター電極の上面より厚みが8mmになるように、造粒粉の充填およびカーボンパンチでの成形をした。 First, a heater laminate was produced. The granulated powder was filled into a bottomed carbon mold and pressed with a carbon punch to produce a molded body with a diameter of Φ320 mm and a thickness of 8 mm. Next, a heater electrode was placed on the molded body. The heater electrode was a Mo mesh (wire diameter 0.1 mm, mesh size #50, plain weave) cut into a specified pattern to match the resistance value of the heater electrode. Next, the carbon mold was further filled with granulated powder and the heater electrode was embedded to produce a heater laminate. At this time, the granulated powder was filled and molded with a carbon punch so that the thickness from the top surface of the heater electrode was 8 mm.
次に、板状のMoをヒーター積層体上に載置した。そして、Moを載置したカーボン型に造粒粉をさらに充填してMoを埋設した。このとき、板状のMoの上面より厚みが8mmになるようにカーボンパンチで成形し、積層体を作製した。このようにして、ヒーター積層体、および板状の高融点金属が積層された積層体を作製した。 Next, a plate-shaped Mo was placed on the heater laminate. The carbon mold on which the Mo was placed was further filled with granulated powder to embed the Mo. At this time, the plate-shaped Mo was molded with a carbon punch so that the thickness from the top surface was 8 mm, and a laminate was produced. In this way, a heater laminate and a laminate in which plate-shaped high-melting point metal were stacked were produced.
そして、カーボンパンチをカーボン型に挿入した状態で、温度1800℃、圧力4MPa、N2雰囲気で4時間一軸ホットプレス焼成を行った。焼成後、外形加工(Φ300mm×18mm)を行った。各々の電極と外部電源とを接続するための端子穴の穿設、端子の接続、および必要な絶縁構造の作製は、焼成後の加工時に同時に行なった。このようにして、実施例5の電極埋設部材を作製した。 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 N2 atmosphere for 4 hours. After firing, external processing (Φ300 mm x 18 mm) was performed. Drilling terminal holes for connecting each electrode to an external power source, connecting the terminals, and fabricating the necessary insulating structure were performed simultaneously during processing after firing. In this manner, the electrode-embedded member of Example 5 was fabricated.
(評価)
作製されたヒーターモジュールは、ヒーター電極に外部電源より通電することにより400℃に加熱することができた。
(evaluation)
The manufactured heater module could be heated to 400° C. by passing electricity through the heater electrodes from an external power source.
次に、実施例1の試料について、積層方向に垂直な切断面をEPMAで元素分析をしてマッピングした。図5(a)~(d)は、それぞれ実施例1のEPMAのマッピングを示す写真である。図5(a)は、実施例1の断面の分析視野のSEM画像である。図5(b)~(d)は、それぞれ、Mo、Y、およびOをマッピングした写真である。灰色および白色の部分が、それぞれMo、Y、およびOが検出された部分を示している。 Next, the cut surface of the sample of Example 1 perpendicular to the stacking direction was subjected to elemental analysis and mapping using EPMA. Figures 5(a) to (d) are photographs showing the EPMA mapping of Example 1. Figure 5(a) is an SEM image of the analyzed field of view of the cross section of Example 1. Figures 5(b) to (d) are photographs in which Mo, Y, and O were mapped, respectively. The gray and white areas indicate the areas where Mo, Y, and O were detected, respectively.
図5(a)~(d)に示されるように、Y、およびOは、セラミックス部材(AlN)内にも存在するが、セラミックス部材および高融点の金属部材(Mo)の接合界面にそれより多く存在していることが分かった。すなわち、セラミックス部材および金属部材の接合界面は、セラミックス部材の第2相を構成する金属の濃度および酸素濃度が、セラミックス部材の内部の金属の濃度および酸素濃度よりそれぞれ大きいことが確かめられた。 As shown in Figures 5(a) to (d), it was found that Y and O are present in the ceramic member (AlN), but are present in greater amounts at the bonding interface between the ceramic member and the high-melting-point metal member (Mo). In other words, it was confirmed that at the bonding interface between the ceramic member and the metal member, the metal concentration and oxygen concentration constituting the second phase of the ceramic member are greater than the metal concentration and oxygen concentration, respectively, inside the ceramic member.
本発明の接合体は、セラミックス部材および金属部材の接合界面に、セラミックス部材の第2相を構成する金属および酸素が高濃度で存在することで、これらを介してMoとAlNとの化学結合がされている可能性が高いと考えられる。また、本発明の製造方法は、焼結時にMoの再結晶化温度を越えるため、接合面でのMoの塑性変形によりAlN焼結体の表面の凹凸にMoが侵入しアンカー効果を発揮することで、さらに高い接合強度が得られるものと推定される。 The bonded body of the present invention is likely to have a chemical bond between Mo and AlN due to the high concentration of metal and oxygen that constitute the second phase of the ceramic member at the bonding interface between the ceramic member and the metal member. In addition, the manufacturing method of the present invention exceeds the recrystallization temperature of Mo during sintering, so it is presumed that Mo penetrates into the irregularities on the surface of the AlN sintered body due to plastic deformation of Mo at the bonding surface, exerting an anchor effect, resulting in even higher bonding strength.
以上により、本発明の接合体および電極埋設部材は、接合面の浸食やコンタミネーションを抑制でき、接合強度が強く、金属部材の厚みが厚い接合体および電極埋設部材であることが確かめられた。また、本発明の製造方法は、そのような接合体または電極埋設部材を製造できることが確かめられた。 From the above, it has been confirmed that the bonded body and electrode-embedded member of the present invention are bonded bodies and electrode-embedded members that can suppress erosion and contamination of the bonded surfaces, have strong bond strength, and have thick metal members. It has also been confirmed that the manufacturing method of the present invention can manufacture such bonded bodies or electrode-embedded members.
本発明は上記実施形態に限定されず、本発明の思想と範囲に含まれる様々な変形および均等物に及ぶことはいうまでもない。また、各図面に示された構成要素の構造、形状、数、位置、大きさ等は説明の便宜上のものであり、適宜変更しうる。 The present invention is not limited to the above-described embodiment, and it goes without saying that it covers various modifications and equivalents that fall within the spirit and scope of the present invention. Furthermore, the structure, shape, number, position, size, etc. of the components shown in each drawing are for convenience of explanation and may be changed as appropriate.
10 接合体
12 積層体
20 セラミックス部材
22 造粒粉
30 金属部材
32 一方の主面
34 他方の主面
36 板状の高融点金属
40 電極
50 電極埋設部材
60 カーボン型
70 カーボンパンチ
REFERENCE SIGNS LIST 10 Bonded body 12 Laminated body 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 (5)
前記セラミックス部材は、電極が埋設され、
前記セラミックス部材は、少なくとも前記金属部材の一方の主面に接合され、
前記セラミックス部材は、金属酸化物としてのY 2 O 3 からなる第2相を含み、
前記金属部材は、前記金属部材の一方の主面に垂直な方向の最大厚みが1mm以上であり、
前記セラミックス部材および前記金属部材の接合界面は、前記セラミックス部材の前記第2相を構成する金属の濃度および酸素濃度が、前記セラミックス部材の内部の前記金属の濃度および酸素濃度よりそれぞれ大きいことを特徴とする接合体。 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 high melting point metal having a melting point of 2000°C or more,
The ceramic member has an electrode embedded therein,
The ceramic member is joined to at least one main surface of the metal member,
The ceramic member includes a second phase composed of Y 2 O 3 as 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,
A bonded body characterized in that at a bonding interface between the ceramic member and the metal member, the concentration of the metal constituting the second phase of the ceramic member and the oxygen concentration are greater than the concentration of the metal and the oxygen concentration inside the ceramic member, respectively.
前記金属部材は、前記第4族の金属としてのTiが拡散していることを特徴とする請求項1記載の接合体。 The ceramic member contains Ti as a Group 4 metal,
2. The joint body according to claim 1, wherein Ti as the Group 4 metal is diffused in the metal member.
AlN原料粉に金属酸化物としてのYThe AlN raw powder is mixed with Y as a metal oxide. 22 OO 33 の原料粉を添加した粉末を造粒して造粒粉を作製する工程と、A step of granulating the powder to which the raw material powder is added to produce a granulated powder;
前記造粒粉または前記造粒粉から形成した成形体、および厚み1mm以上の板状の前記高融点金属を、前記板状の高融点金属の一方の主面が積層方向に垂直になるようにカーボン型に積層する工程と、A step of stacking the granulated powder or a compact formed from the granulated powder and the plate-shaped high-melting point metal having a thickness of 1 mm or more on a carbon mold such that one main surface of the plate-shaped high-melting point metal is perpendicular to a stacking direction;
前記成形体に電極を埋設する、又は、前記電極を前記成形体で挟むように前記カーボン型に積層する工程と、embedding an electrode in the molded body or stacking the electrode on the carbon mold so as to sandwich the electrode between the molded bodies;
前記カーボン型にカーボンパンチを挿入し、積層体を形成する工程と、inserting a carbon punch into the carbon mold to form a laminate;
前記積層体を一軸加圧焼成する工程と、を含むことを特徴とする接合体の製造方法。and a step of uniaxially pressurizing and sintering the laminate.
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| JP2004087392A (en) | 2002-08-28 | 2004-03-18 | Toshiba Ceramics Co Ltd | AlN heater and method for manufacturing the same |
| JP2005019067A (en) | 2003-06-24 | 2005-01-20 | Toshiba Ceramics Co Ltd | Aluminum nitride ceramic heater |
| JP2005159334A (en) | 2003-10-31 | 2005-06-16 | Tokuyama Corp | Aluminum nitride joined body and manufacturing method thereof |
| JP2006286646A (en) | 2006-04-04 | 2006-10-19 | Sumitomo Electric Ind Ltd | Ceramic heater |
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| JPH0551273A (en) * | 1991-08-22 | 1993-03-02 | Murata Mfg Co Ltd | Joined body of aluminum nitride substrate and metallic sheet |
| JP2967024B2 (en) * | 1994-03-29 | 1999-10-25 | 日本碍子株式会社 | Embedded electrode product and method of manufacturing the same |
| JP3288922B2 (en) * | 1996-03-14 | 2002-06-04 | 日本碍子株式会社 | Joint body and method of manufacturing the same |
| US5932043A (en) * | 1997-03-18 | 1999-08-03 | International Business Machines Corporation | Method for flat firing aluminum nitride/tungsten electronic modules |
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| JP2004087392A (en) | 2002-08-28 | 2004-03-18 | Toshiba Ceramics Co Ltd | AlN heater and method for manufacturing the same |
| JP2005019067A (en) | 2003-06-24 | 2005-01-20 | Toshiba Ceramics Co Ltd | Aluminum nitride ceramic heater |
| JP2005159334A (en) | 2003-10-31 | 2005-06-16 | Tokuyama Corp | Aluminum nitride joined body and manufacturing method thereof |
| JP2006286646A (en) | 2006-04-04 | 2006-10-19 | Sumitomo Electric Ind Ltd | Ceramic heater |
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