JP2022012992A - MANUFACTURING METHOD OF AlN SINTERED MEMBER, MANUFACTURING METHOD OF ELECTRODE EMBEDDING MEMBER, AND ELECTRODE EMBEDDING MEMBER - Google Patents

MANUFACTURING METHOD OF AlN SINTERED MEMBER, MANUFACTURING METHOD OF ELECTRODE EMBEDDING MEMBER, AND ELECTRODE EMBEDDING MEMBER Download PDF

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JP2022012992A
JP2022012992A JP2020115207A JP2020115207A JP2022012992A JP 2022012992 A JP2022012992 A JP 2022012992A JP 2020115207 A JP2020115207 A JP 2020115207A JP 2020115207 A JP2020115207 A JP 2020115207A JP 2022012992 A JP2022012992 A JP 2022012992A
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JP7521783B2 (en
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裕明 鈴木
Hiroaki Suzuki
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Niterra Co Ltd
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NGK Spark Plug Co Ltd
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Abstract

To provide a manufacturing method of an AlN sintered member having improved dimensional accuracy, and an electrode embedding member having high thickness uniformity of an isolation layer and high physical properties.SOLUTION: A method includes the steps of: forming a first and a second AlN compact from an AlN raw material powder; preparing a first and a second AlN degreased body by degreasing the first and the second AlN compact at a temperature higher than or equal to a predetermined temperature for a period longer than or equal to a predetermined time; preparing a first and a second AlN calcined body by calcining the first and the second AlN degreased body; forming a first or a second plain face for the first and the second AlN calcined body; forming a recess at least on one of the first or the second plain face; laminating the first AlN calcined body and the second AlN calcined body with the first plain face being in contact with the second plain face; and firing the first AlN calcined body and the second AlN calcined body having been laminated together while applying a pressure of 10 kgf/cm2 or higher in a lamination direction.SELECTED DRAWING: Figure 1

Description

本発明は、ＡｌＮ焼結部材の製造方法、電極埋設部材の製造方法および電極埋設部材に関する。 The present invention relates to a method for manufacturing an AlN sintered member, a method for manufacturing an electrode-embedded member, and an electrode-embedded member.

半導体製造装置において、ウエハなどの基板を表面に保持するセラミック製静電チャックは、基板載置面とセラミックスに埋設されている静電吸着用電極や高周波電極までの離間距離、すなわち絶縁層の厚みを均一にすることが要求されている。そしてこのようなセラミックス素材として、ＡｌＮ（窒化アルミニウム）焼結体が用いられている。 In semiconductor manufacturing equipment, the ceramic electrostatic chuck that holds a substrate such as a wafer on the surface is the separation distance between the substrate mounting surface and the electrostatic adsorption electrode or high frequency electrode embedded in the ceramics, that is, the thickness of the insulating layer. Is required to be uniform. As such a ceramic material, an AlN (aluminum nitride) sintered body is used.

しかしながら、ＡｌＮ焼結体は焼結温度が高く、難焼結性であり、かつ、金属電極をＡｌＮ焼結体中に埋設するにはホットプレス焼成など手段が限られていた。 However, the AlN sintered body has a high sintering temperature and is difficult to sinter, and means such as hot press firing are limited for embedding the metal electrode in the AlN sintered body.

なお、特許文献１には、セラミックス仮焼体同士を通常の焼成温度より高い温度で常圧、荷重下で焼成することにより、一体化する技術が開示されている。ただし、錘を載置した荷重下でアルミナの仮焼体同士及びムライトの仮焼体同士を一体化した実施例しか挙げられておらず、ＡｌＮ仮焼体を一体化する実施例は挙げられていない。 In addition, Patent Document 1 discloses a technique of integrating ceramic calcined bodies by firing them at a temperature higher than a normal firing temperature under normal pressure and load. However, only the examples in which the alumina calcined bodies and the mullite calcined bodies are integrated under the load on which the weight is placed are given, and the examples in which the AlN calcined bodies are integrated are mentioned. do not have.

また、特許文献２には、２つの被焼結体をホットプレス成形することにより厚さの異なるセラミックス焼結体を得る技術が開示されている。被焼結体には、セラミックス粉末、セラミックス成形体、セラミックス脱脂体及びセラミックス焼結体が含まれるとされている。成形型上に形成された成形体の上に金属部材を載せ、その上に粉末を収容しホットプレス焼成する技術が開示されている。 Further, Patent Document 2 discloses a technique for obtaining ceramic sintered bodies having different thicknesses by hot-press molding two sintered bodies. The sintered body is said to include a ceramic powder, a ceramic molded body, a ceramic degreased body, and a ceramic sintered body. A technique of placing a metal member on a molded body formed on a molding die, accommodating powder on the metal member, and hot-press firing is disclosed.

また、特許文献３には、冷間等方圧加圧法（ＣＩＰ）によりセラミックス成形体を成形し、セラミックス成形体に形成した溝内に電極を収容し、複数のセラミックス成形体を重ね合わせ、重ね合わせ方向に加圧しながら焼成することにより、電極が内蔵されたセラミックス焼成体を製造する技術が開示されている。 Further, in Patent Document 3, a ceramic molded body is molded by a cold isotropic pressure method (CIP), an electrode is housed in a groove formed in the ceramic molded body, and a plurality of ceramic molded bodies are superposed and stacked. A technique for manufacturing a ceramic fired body having a built-in electrode by firing while pressurizing in the mating direction is disclosed.

特開平６－２９８５７４号公報Japanese Unexamined Patent Publication No. 6-298574 特開２０００－１４１３３６号公報Japanese Unexamined Patent Publication No. 2000-141336 特許６１４８８４５号公報Japanese Patent No. 6148845

しかしながら、上記特許文献１に記載された技術では、実際にはＡｌＮ仮焼体同士を焼成しても一体化することはできないという課題があった。また、特許文献２、３に記載された技術では、セラミックス中に電極等が埋設された部材を製造した際、その各部寸法精度にバラツキがみられる。たとえば、セラミックスからなる絶縁層の厚みの均一性が要求される場合や絶縁層自体の物性を製造条件で調節することは困難であり、特に所定の電気的特性を要求される電極埋設部材の製法としては適当でないという課題があった。 However, the technique described in Patent Document 1 has a problem that the AlN calcined bodies cannot be integrated even if they are actually fired. Further, in the techniques described in Patent Documents 2 and 3, when a member in which an electrode or the like is embedded in ceramics is manufactured, the dimensional accuracy of each part varies. For example, when the uniformity of the thickness of the insulating layer made of ceramics is required, or it is difficult to adjust the physical properties of the insulating layer itself under the manufacturing conditions, a method for manufacturing an electrode embedded member which requires predetermined electrical characteristics in particular. There was a problem that it was not appropriate.

本発明は、このような事情に鑑みてなされたものであり、寸法精度の向上したＡｌＮ焼結部材の製造方法、および絶縁層の厚みの均一性が高く物性が調整された電極埋設部材を提供することを目的とする。 INDUSTRIAL APPLICABILITY The present invention has been made in view of such circumstances, and provides a method for manufacturing an AlN sintered member with improved dimensional accuracy, and an electrode-embedded member having a highly uniform thickness of an insulating layer and adjusted physical properties. The purpose is to do.

（１）上記の目的を達成するため、本発明のＡｌＮ焼結部材の製造方法は、ＡｌＮを主成分とするＡｌＮ焼結部材の製造方法であって、ＡｌＮ原料粉から第１および第２のＡｌＮ成形体を形成する工程と、前記第１および第２のＡｌＮ成形体を所定の温度以上、所定の時間以上脱脂処理して第１および第２のＡｌＮ脱脂体を作製する工程と、前記第１および第２のＡｌＮ脱脂体を仮焼して第１および第２のＡｌＮ仮焼体を作製する工程と、前記第１のＡｌＮ仮焼体に第１の平面を形成する工程と、前記第２のＡｌＮ仮焼体に第２の平面を形成する工程と、前記第１の平面または前記第２の平面の少なくとも一方に凹部を形成する工程と、前記第１のＡｌＮ仮焼体と前記第２のＡｌＮ仮焼体とを、前記第１の平面と前記第２の平面とを接触させた状態で積層する工程と、前記積層した前記第１のＡｌＮ仮焼体および前記第２のＡｌＮ仮焼体を、積層方向に１０ｋｇｆ／ｃｍ２以上の圧力を加えながら焼成する工程と、を備えることを特徴としている。 (1) In order to achieve the above object, the method for producing an AlN sintered member of the present invention is a method for producing an AlN sintered member containing AlN as a main component, and is the first and second methods for producing an AlN raw material powder. A step of forming an AlN molded body, a step of degreasing the first and second AlN molded bodies at a predetermined temperature or higher and a predetermined time or longer to produce first and second AlN degreased bodies, and the first step. A step of calcining the first and second AlN degreased bodies to prepare first and second AlN calcined bodies, a step of forming a first plane on the first AlN calcined body, and the first step. A step of forming a second plane in the AlN calcined body of 2, a step of forming a recess in at least one of the first plane or the second plane, and the first AlN calcined body and the first. The step of laminating the AlN calcined body of 2 in a state where the first plane and the second plane are in contact with each other, and the laminated first AlN calcined body and the second AlN temporary calcined body. It is characterized by comprising a step of firing the fired body while applying a pressure of 10 kgf / cm 2 or more in the laminating direction.

本発明のＡｌＮ焼結部材の製造方法によれば、凹部に由来する中空構造を有するＡｌＮ焼結部材を得ることが可能となる。第１および第２のＡｌＮ仮焼体に第１および第２の平面並びに凹部を形成しているが、これらを形成するための研削や研磨などの作業は、ＡｌＮ焼結体にこれらを形成する場合と比較して、作業時間の短縮化を図ることが可能となる。また、凹部を形成したＡｌＮ成形体同士を焼成して一体化する場合と比較して、凹部に由来するＡｌＮ焼結部材の外形および中空構造の寸法精度の向上を図ることが可能となる。また、錘を用いた小さな荷重を加えた状態で焼成を行う上記特許文献１に開示された技術と比較して、１０ｋｇｆ／ｃｍ２（＝０．９８ＭＰａ）以上の加圧を行いながら焼成を行うので、接合強度の向上、およびＡｌＮ焼結部材の緻密化を図ることが可能となる。 According to the method for manufacturing an AlN sintered member of the present invention, it is possible to obtain an AlN sintered member having a hollow structure derived from a recess. The first and second planes and recesses are formed on the first and second AlN calcined bodies, but the work such as grinding and polishing to form these is formed on the AlN sintered body. Compared with the case, it is possible to shorten the working time. Further, it is possible to improve the dimensional accuracy of the outer shape and the hollow structure of the AlN sintered member derived from the concave portion as compared with the case where the AlN molded bodies having the concave portions are fired and integrated. Further, as compared with the technique disclosed in Patent Document 1 above, in which firing is performed in a state where a small load is applied using a weight, firing is performed while applying a pressure of 10 kgf / cm 2 (= 0.98 MPa) or more. Therefore, it is possible to improve the bonding strength and to densify the AlN sintered member.

（２）また、本発明のＡｌＮ焼結部材の製造方法において、前記第１および第２のＡｌＮ仮焼体を作製する工程の仮焼温度は、１２００℃以上１７００℃以下であり、かつ、前記焼成する工程の焼成温度は、１８００℃以上２０００℃以下であることを特徴としている。これにより、ＡｌＮ焼結部材を形成する各層の接合強度が強くなる。 (2) Further, in the method for manufacturing an AlN sintered member of the present invention, the calcining temperature in the steps of producing the first and second AlN calcined bodies is 1200 ° C. or higher and 1700 ° C. or lower, and the above-mentioned The firing temperature in the firing step is 1800 ° C. or higher and 2000 ° C. or lower. As a result, the bonding strength of each layer forming the AlN sintered member is increased.

（３）また、本発明のＡｌＮ焼結部材の製造方法は、前記第１のＡｌＮ仮焼体と前記第２のＡｌＮ仮焼体とを積層する工程において、前記凹部の少なくとも一部に電極を配置して積層することを特徴としている。これにより、電極が埋設されたＡｌＮ焼結部材の寸法精度の向上を図ることが可能となる。例えば、ＡｌＮ焼結部材の絶縁層となる層の厚みの寸法精度を向上させると、絶縁層の厚みのバラツキを低減させることができる。 (3) Further, in the method for manufacturing an AlN sintered member of the present invention, in the step of laminating the first AlN calcined body and the second AlN calcined body, an electrode is provided in at least a part of the recess. It is characterized by arranging and stacking. This makes it possible to improve the dimensional accuracy of the AlN sintered member in which the electrodes are embedded. For example, if the dimensional accuracy of the thickness of the layer to be the insulating layer of the AlN sintered member is improved, the variation in the thickness of the insulating layer can be reduced.

（４）また、本発明のＡｌＮ焼結部材の製造方法において、前記第１または第２のＡｌＮ成形体を形成する前記ＡｌＮ原料粉は、少なくとも一方にＹ成分が添加され、前記第１および第２のＡｌＮ脱脂体を作製する工程において、Ｙ成分が添加された前記第１または第２のＡｌＮ成形体は、脱脂温度Ｔ（℃）と脱脂時間Ｈ（ｈ）と添加したＹ成分をＹ２Ｏ３換算した内比でＣ（ｗｔ％）として、Ｔ＞２０×Ｃ＋４４０かつＨ≧３００／｛Ｔ－（２０×Ｃ＋４４０）｝を満たす条件で前記第１または第２のＡｌＮ脱脂体が作製されることを特徴としている。これにより、電極が埋設されたＡｌＮ焼結部材の少なくとも一部の焼結体の体積抵抗率を相対的に低い値に調整することができる。例えば、ＡｌＮ焼結部材が静電チャックとして使用される場合、絶縁層の体積抵抗率を低い値に調整することにより、処理対象に対し強い静電吸着力を発揮できる。 (4) Further, in the method for producing an AlN sintered member of the present invention, the AlN raw material powder forming the first or second AlN molded body is added with a Y component to at least one of the first and second AlN raw materials. In the step of producing the AlN degreased body of 2, the first or second AlN molded body to which the Y component was added has a degreasing temperature T (° C.), a degreasing time H (h), and a Y component added to Y 2 . The first or second AlN degreased body is produced under the condition that T> 20 × C + 440 and H ≧ 300 / {T- (20 × C + 440)} as C (wt%) in the internal ratio converted to O3. It is characterized by that. Thereby, the volume resistivity of at least a part of the sintered body of the AlN sintered member in which the electrode is embedded can be adjusted to a relatively low value. For example, when the AlN sintered member is used as an electrostatic chuck, a strong electrostatic adsorption force can be exerted on the object to be treated by adjusting the volume resistivity of the insulating layer to a low value.

（５）また、本発明の電極埋設部材は、一体に形成され、処理対象を表面上に保持する電極埋設部材であって、ＡｌＮを主成分とするセラミックス焼結体で形成された絶縁層およびバルク層と、前記絶縁層とバルク層との間に設けられた電極と、を備え、前記絶縁層の厚みのバラツキは７５μｍ以下であることを特徴としている。このように絶縁層の厚みのバラツキが低減されていることにより、例えば、電極埋設部材が静電チャックとして使用される場合、面内の吸着力の差を低減することができる。また、例えば、ウエハ加熱用ヒーターとして用いられる場合、面内の温度のバラツキを低減することができる。 (5) Further, the electrode-embedded member of the present invention is an electrode-embedded member that is integrally formed and holds a processing target on the surface, and is an insulating layer formed of a ceramic sintered body containing AlN as a main component and an insulating layer. It comprises a bulk layer and an electrode provided between the insulating layer and the bulk layer, and is characterized in that the thickness variation of the insulating layer is 75 μm or less. By reducing the variation in the thickness of the insulating layer in this way, for example, when the electrode embedded member is used as an electrostatic chuck, it is possible to reduce the difference in the suction force in the plane. Further, for example, when it is used as a heater for heating a wafer, it is possible to reduce in-plane temperature variation.

（６）また、本発明の電極埋設部材において、前記絶縁層は、前記セラミックス焼結体のＡｌＮ粒界にＹＡＧ粒子が含まれ、ＹＡＰ粒子およびＹＡＭ粒子が含まれないことを特徴としている。これにより、絶縁層の体積抵抗率を小さい範囲で調整することができ、例えば、電極埋設部材が静電チャックとして使用される場合、処理対象に対し強い静電吸着力を発揮できる。 (6) Further, in the electrode-embedded member of the present invention, the insulating layer is characterized in that YAG particles are contained in the AlN grain boundaries of the ceramic sintered body, and YAP particles and YAM particles are not contained. Thereby, the volume resistivity of the insulating layer can be adjusted in a small range. For example, when the electrode embedded member is used as an electrostatic chuck, a strong electrostatic adsorption force can be exerted on the object to be processed.

（７）また、本発明の電極埋設部材は、さらに、前記処理対象を保持する表面と対向する面にＡｌＮを主成分とするセラミックス焼結体で形成された支持部材が接合されていることを特徴としている。これにより、電極埋設部材をシャフト付きヒーター等に適用することができる。 (7) Further, in the electrode-embedded member of the present invention, a support member formed of a ceramic sintered body containing AlN as a main component is further bonded to a surface facing the surface holding the object to be treated. It is a feature. Thereby, the electrode embedded member can be applied to a heater with a shaft or the like.

本発明の第１および第２の実施形態に係るＡｌＮ焼結部材の製造方法を示すフローチャートである。It is a flowchart which shows the manufacturing method of the AlN sintered member which concerns on 1st and 2nd Embodiment of this invention. （ａ）～（ｄ）それぞれ第１の実施形態の製造工程の一段階を模式的に示す断面図である。It is sectional drawing which shows typically one step of the manufacturing process of 1st Embodiment, each of (a)-(d). （ａ）～（ｄ）それぞれ第２の実施形態の製造工程の一段階を模式的に示す断面図である。It is sectional drawing which shows typically one step of the manufacturing process of 2nd Embodiment in each of (a)-(d). Ｙ成分の添加量としきい式の関係を例示した図である。It is a figure which exemplifies the relationship between the addition amount of the Y component and the threshold formula. 第２の実施形態に係る電極埋設部材を模式的に示す正断面図である。It is a front sectional view schematically showing the electrode embedded member which concerns on 2nd Embodiment. 第２の実施形態に係る電極埋設部材を模式的に示す正断面図である。It is a front sectional view schematically showing the electrode embedded member which concerns on 2nd Embodiment. 各試料の製造条件および評価結果を示す表である。It is a table which shows the manufacturing condition and evaluation result of each sample. 各試料の製造条件および評価結果を示す表である。It is a table which shows the manufacturing condition and evaluation result of each sample.

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. In order to facilitate understanding of the description, the same reference number is assigned to the same component in each drawing, and duplicate description is omitted. In the configuration diagram, the size of each component is conceptually represented, and does not necessarily represent the actual dimensional ratio.

［第１の実施形態］
（ＡｌＮ焼結部材の製造方法）
図１は、本発明の第１および第２の実施形態に係るＡｌＮ焼結部材の製造方法を示すフローチャートである。本発明の第１の実施形態に係るＡｌＮ焼結部材１０の製造方法は、図１に示すように、第１および第２のＡｌＮ成形体形成工程ＳＴＥＰ１、第１および第２のＡｌＮ脱脂体作製工程ＳＴＥＰ２、第１および第２のＡｌＮ仮焼体作製工程ＳＴＥＰ３、第１の平面形成工程ＳＴＥＰ４、第２の平面形成工程ＳＴＥＰ５、凹部形成工程ＳＴＥＰ６、積層工程ＳＴＥＰ７および焼成工程ＳＴＥＰ８を備えている。 [First Embodiment]
(Manufacturing method of AlN sintered member)
FIG. 1 is a flowchart showing a method for manufacturing an AlN sintered member according to the first and second embodiments of the present invention. As shown in FIG. 1, the method for manufacturing the AlN sintered member 10 according to the first embodiment of the present invention is the first and second AlN molded body forming steps STEP 1, the first and second AlN degreased body preparation. It includes a step STEP2, a first and second AlN calcined body manufacturing step STEP3, a first plane forming step STEP4, a second plane forming step STEP5, a recess forming step STEP6, a laminating step STEP7, and a firing step STEP8.

図２（ａ）～（ｄ）は、それぞれ本実施形態の製造工程の一段階を模式的に示す断面図である。第１および第２のＡｌＮ成形体形成工程ＳＴＥＰ１では、ＡｌＮ原料粉から第１および第２のＡｌＮ成形体１１、１２を形成する。例えば、ＡｌＮ粉末に焼結助剤、熱硬化性樹脂バインダなどの添加剤を適宜添加して混合して、ＡｌＮ原料粉を作製し、顆粒を造粒後、加圧成形してＡｌＮ成形体を形成することができる。 2 (a) to 2 (d) are cross-sectional views schematically showing one step of the manufacturing process of the present embodiment, respectively. In the first and second AlN molded body forming steps STEP1, the first and second AlN molded bodies 11 and 12 are formed from the AlN raw material powder. For example, an additive such as a sintering aid and a thermosetting resin binder is appropriately added to the AlN powder and mixed to prepare an AlN raw material powder, and after granulating the granules, pressure molding is performed to obtain an AlN molded product. Can be formed.

ＡｌＮ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。 The AlN powder is preferably of high purity, 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, and more preferably 0.3 μm or more and 0.8 μm or less.

混合方法は、湿式、乾式の何れであってもよく、例えばボールミル、振動ミルなどの混合器を用いることができる。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。 The mixing method may be either wet or dry, and for example, a mixer such as a ball mill or a vibration mill can be used. As the molding method, for example, a known method such as uniaxial pressure molding or cold isostatic pressing (CIP) method may be used.

第１および第２のＡｌＮ脱脂体作製工程ＳＴＥＰ２では、第１および第２のＡｌＮ成形体１１、１２を所定の温度以上、所定の時間以上脱脂処理して第１および第２のＡｌＮ脱脂体２１、２２を作製する。ＡｌＮ成形体は、例えば、４００℃以上８００℃以下の温度で熱処理され、ＡｌＮ脱脂体となる。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。脱脂には、大気炉または窒素雰囲気炉を用いることができるが、バインダの有機成分を除去することが重要なので大気炉の方が好ましい。なお、第１および第２のＡｌＮ脱脂体作製工程ＳＴＥＰ２において、第１および第２のＡｌＮ成形体の脱脂温度および脱脂時間は同じであっても、相違していてもよい。 In the first and second AlN degreasing body manufacturing steps STEP2, the first and second AlN molded bodies 11 and 12 are degreased at a predetermined temperature or higher and for a predetermined time or longer, and the first and second AlN degreasing bodies 21 are subjected to degreasing treatment. , 22 is produced. The AlN molded product is, for example, heat-treated at a temperature of 400 ° C. or higher and 800 ° C. or lower to become an AlN degreased product. The degreasing time is preferably 1 hour or more and 120 hours or less. An atmospheric furnace or a nitrogen atmosphere furnace can be used for degreasing, but the atmosphere furnace is preferable because it is important to remove the organic component of the binder. In the first and second AlN degreasing body manufacturing steps STEP2, the degreasing temperature and the degreasing time of the first and second AlN molded bodies may be the same or different.

第１および第２のＡｌＮ仮焼体作製工程ＳＴＥＰ３では、第１および第２のＡｌＮ脱脂体２１、２２を１２００℃以上１７００℃以下の温度で仮焼して第１および第２のＡｌＮ仮焼体３１、３２を作製する。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。なお、第１および第２のＡｌＮ仮焼体作製工程ＳＴＥＰ３において、第１および第２のＡｌＮ脱脂体の仮焼温度および仮焼時間は同じであっても、相違していてもよい。 In the first and second AlN calcined body preparation steps STEP3, the first and second AlN degreased bodies 21 and 22 are calcined at a temperature of 1200 ° C. or higher and 1700 ° C. or lower, and the first and second AlN calcined bodies are calcined. The bodies 31 and 32 are made. The calcination time is preferably 0.5 hours or more and 12 hours or less. The calcination atmosphere is preferably a nitrogen or inert gas atmosphere, but may be a vacuum or the like. In the first and second AlN calcined body preparation step STEP3, the calcining temperature and the calcining time of the first and second AlN degreased bodies may be the same or different.

第１の平面形成工程ＳＴＥＰ４では、第１のＡｌＮ仮焼体３１に第１の平面３１ａとその反対面３１ｂを形成する。第２の平面形成工程ＳＴＥＰ５では、第２のＡｌＮ仮焼体３２に第２の平面３２ａとその反対面３２ｂを形成する。なお、第１の平面３１ａと第２の平面３２ａは、積層工程ＳＴＥＰ７において接触する面となる。 In the first plane forming step STEP4, the first plane 31a and the opposite surface 31b are formed on the first AlN calcined body 31. In the second plane forming step STEP5, the second plane 32a and the opposite surface 32b are formed on the second AlN calcined body 32. The first plane 31a and the second plane 32a are surfaces that come into contact with each other in the laminating step STEP7.

ＮＣ旋盤、ＭＣ加工機などの平面研削機やラッピング加工機などを用いて、例えば、表面粗さＲａが、好ましくは０．１５μｍ以上０．８μｍ以下、より好ましくは０．１５μｍ以上０．４μｍ以下となるように研磨または研削を行うことにより、第１および第２の平面３１ａ、３２ａを形成する。 Using a surface grinder such as an NC lathe or MC processing machine or a lapping processing machine, for example, the surface roughness Ra is preferably 0.15 μm or more and 0.8 μm or less, more preferably 0.15 μm or more and 0.4 μm or less. The first and second flat surfaces 31a and 32a are formed by polishing or grinding so as to be.

凹部形成工程ＳＴＥＰ６においては、第１の平面３１ａまたは第２の平面３２ａの少なくとも一方に凹部３３を形成する。凹部３３は、第１の平面３１ａ、第２の平面３２ａの何れか一方、または双方から掘り込むように研削加工などによって形成する。 In the recess forming step STEP6, the recess 33 is formed on at least one of the first plane 31a and the second plane 32a. The recess 33 is formed by grinding or the like so as to be dug from either or both of the first flat surface 31a and the second flat surface 32a.

なお、第１の平面形成工程ＳＴＥＰ４または第２の平面形成工程ＳＴＥＰ５において、第１または第２の平面３１ａ、３２ａを研磨加工せずに、あるいは粗く研削加工しただけとしておき、凹部形成工程ＳＴＥＰ５において凹部３３を形成した後で、第１または第２の平面３１ａ、３２ａを研磨加工、あるいは仕上げの研削加工を行ってもよい。 In the first flat surface forming step STEP4 or the second flat surface forming step STEP5, the first or second flat surfaces 31a and 32a are left unpolished or only roughly ground, and in the concave portion forming step STEP5. After forming the recess 33, the first or second flat surfaces 31a and 32a may be polished or finished by grinding.

なお、第１および第２の平面３１ａ、３２ａの双方から掘り込むように凹部３３を形成する場合、これらの凹部３３は、第１および第２の平面３１ａ、３２ａを積層工程ＳＴＥＰ６において接触されたときに、一体化するものであってもよいが、他の平面によって閉じられるものであってもよい。 When the recesses 33 are formed so as to be dug from both the first and second planes 31a and 32a, these recesses 33 are brought into contact with the first and second planes 31a and 32a in the laminating step STEP6. Sometimes it may be integrated, but it may also be closed by another plane.

また、第１の平面形成工程ＳＴＥＰ４、第２の平面形成工程ＳＴＥＰ５または凹部形成工程ＳＴＥＰ６において、乾式の研削加工または研磨加工により、第１の平面３１ａ、第２の平面３２ａまたは凹部３３を形成することが好ましい。これにより、研削液又は研磨液が第１または第２のＡｌＮ仮焼体３１、３２の内部に侵入し、ＡｌＮ焼結部材１０に不純物が残存するおそれの解消を図ることが可能となる。なお、研削加工および研磨加工を行う場合、これら加工の双方ともに乾式で行うことが好ましい。 Further, in the first flat surface forming step STEP4, the second flat surface forming step STEP5 or the concave portion forming step STEP6, the first flat surface 31a, the second flat surface 32a or the concave portion 33 is formed by dry grinding or polishing. Is preferable. This makes it possible to eliminate the possibility that the grinding liquid or the polishing liquid invades the inside of the first or second AlN calcined bodies 31 and 32 and impurities remain in the AlN sintered member 10. When performing grinding and polishing, it is preferable to perform both of these processes in a dry manner.

積層工程ＳＴＥＰ７では、第１のＡｌＮ仮焼体３１と第２のＡｌＮ仮焼体３２とを、第１の平面３１ａと第２の平面３２ａとを接触させた状態で積層する。 In the laminating step STEP7, the first AlN calcined body 31 and the second AlN calcined body 32 are laminated in a state where the first flat surface 31a and the second flat surface 32a are in contact with each other.

焼成工程ＳＴＥＰ８では、積層した第１のＡｌＮ仮焼体３１および第２のＡｌＮ仮焼体３２を、積層方向に１０ｋｇｆ／ｃｍ２以上の圧力を加えながら１８００℃以上２０００℃以下で焼成する。これにより、第１および第２のＡｌＮ仮焼体３１、３２が焼結して、それぞれ第１および第２のＡｌＮ焼結体４１、４２となり、これらが一体化されたＡｌＮ焼結部材１０が得られる。 In the firing step STEP8, the laminated first AlN calcined body 31 and the second AlN calcined body 32 are fired at 1800 ° C. or higher and 2000 ° C. or lower while applying a pressure of 10 kgf / cm 2 or more in the laminating direction. As a result, the first and second AlN calcined bodies 31 and 32 are sintered to become the first and second AlN sintered bodies 41 and 42, respectively, and the AlN sintered member 10 in which these are integrated is formed. can get.

焼成工程ＳＴＥＰ８においては、少なくとも積層方向に加圧した状態で加熱するホットプレスなどによって、加圧焼結を行う。加熱時間は、好ましくは０．１時間以上１０時間以下、より好ましくは１時間以上５時間以下である。そして、焼成雰囲気は、例えば、窒素や不活性ガス雰囲気であるが、真空などの雰囲気であってもよい。 In the firing step STEP8, pressure sintering is performed by a hot press or the like that heats at least in a state of being pressurized in the stacking direction. The heating time is preferably 0.1 hour or more and 10 hours or less, and more preferably 1 hour or more and 5 hours or less. The firing atmosphere is, for example, a nitrogen or inert gas atmosphere, but may be a vacuum or the like.

上述した本発明のＡｌＮ焼結部材１０の製造方法においては、凹部を形成したＡｌＮ成形体同士を焼成して一体化する場合と比較して、凹部３３に由来するＡｌＮ焼結部材１０の外形および中空構造などの寸法精度の向上を図ることが可能となる。ＡｌＮ焼結部材に形成される中空構造は電極の配置スペースやガス流路、熱電対などの配線用の空間として利用される。 In the method for manufacturing the AlN sintered member 10 of the present invention described above, the outer shape of the AlN sintered member 10 derived from the recess 33 and the outer shape of the AlN sintered member 10 derived from the recess 33 are compared with the case where the AlN molded bodies having the recess formed are fired and integrated. It is possible to improve the dimensional accuracy of hollow structures and the like. The hollow structure formed in the AlN sintered member is used as a space for arranging electrodes, a gas flow path, a space for wiring such as a thermocouple, and the like.

さらに、錘を用いた小さな荷重を加えた状態で焼成を行う上記特許文献１に開示された技術と比較して、１０ｋｇｆ／ｃｍ２以上の加圧を行いながら焼成を行うので、接合強度の向上、およびＡｌＮ焼結部材１０の緻密化を図ることが可能となる。なお、１０ｋｇｆ／ｃｍ２未満の加圧では、焼成時に第１及び第２のＡｌＮ仮焼体３１、３２の第１および第２の平面３１ａ、３２ａの良好な面接触が得られず接合不良を引き起こすため不適である。 Further, as compared with the technique disclosed in Patent Document 1 in which firing is performed with a small load applied using a weight, firing is performed while applying a pressure of 10 kgf / cm 2 or more, so that the bonding strength is improved. , And the AlN sintered member 10 can be densified. If the pressure is less than 10 kgf / cm 2 , good surface contact between the first and second flat surfaces 31a and 32a of the first and second AlN calcined bodies 31 and 32 cannot be obtained at the time of firing, resulting in poor joining. Not suitable for causing.

［第２の実施形態］
（電極埋設部材の製造方法）
次に、本発明の第２の実施形態に係るＡｌＮ焼結部材の製造方法について説明する。本実施形態に係るＡｌＮ焼結部材の製造方法は、積層工程において、電極を配置して積層するため、電極が埋設されたＡｌＮ焼結部材（電極埋設部材）となる。このような電極埋設部材は、例えば、静電チャックやウエハ加熱用ヒーターとして使用される。また、さらに脱脂条件を調節してＡｌＮ脱脂体を作製することができる。ここで、脱脂条件を下記に示す条件とすることにより、静電チャックとしての機能をより高く発揮させることができる。 [Second Embodiment]
(Manufacturing method of electrode embedded member)
Next, a method for manufacturing the AlN sintered member according to the second embodiment of the present invention will be described. In the method for manufacturing an AlN sintered member according to the present embodiment, since the electrodes are arranged and laminated in the laminating step, the AlN sintered member (electrode embedded member) in which the electrodes are embedded is used. Such an electrode-embedded member is used, for example, as an electrostatic chuck or a wafer heating heater. Further, the degreasing conditions can be further adjusted to produce an AlN degreased body. Here, by setting the degreasing condition as the condition shown below, the function as an electrostatic chuck can be exhibited more highly.

本発明の第２の実施形態に係るＡｌＮ焼結部材（電極埋設部材）５０の製造方法は、図１に示すように、第１および第２のＡｌＮ成形体形成工程ＳＴＥＰ１、第１および第２のＡｌＮ脱脂体作製工程ＳＴＥＰ２、第１および第２のＡｌＮ仮焼体作製工程ＳＴＥＰ３、第１の平面形成工程ＳＴＥＰ４、第２の平面形成工程ＳＴＥＰ５、凹部形成工程ＳＴＥＰ６、積層工程ＳＴＥＰ７および焼成工程ＳＴＥＰ８を備えている。本実施形態に係るＡｌＮ焼結部材の製造方法は、第１の実施形態に係るＡｌＮ焼結部材の製造方法と同様の方法で製造されるため、以下では、第１の実施形態に係るＡｌＮ焼結部材の製造方法と異なる点を説明する。 As shown in FIG. 1, the method for manufacturing the AlN sintered member (electrode embedded member) 50 according to the second embodiment of the present invention is the first and second AlN molded body forming steps STEP1, the first and the second. AlN degreased body manufacturing process STEP2, first and second AlN calcined body manufacturing process STEP3, first plane forming step STEP4, second plane forming step STEP5, recess forming step STEP6, laminating step STEP7 and firing step STEP8 It is equipped with. Since the method for manufacturing the AlN sintered member according to the present embodiment is the same as the method for manufacturing the AlN sintered member according to the first embodiment, the following describes the AlN firing according to the first embodiment. The difference from the manufacturing method of the connecting member will be described.

図３（ａ）～（ｄ）は、それぞれ本実施形態の製造工程の一段階を模式的に示す断面図である。積層工程ＳＴＥＰ７では、凹部形成工程ＳＴＥＰ６で形成した凹部３３の少なくとも一部に電極１５０を配置した後に、第１のＡｌＮ仮焼体３１と第２のＡｌＮ仮焼体３２とを、第１の平面３１ａと第２の平面３２ａとを接触させた状態で積層する。これにより、電極１５０が埋設されたＡｌＮ焼結部材５０となる。 3 (a) to 3 (d) are cross-sectional views schematically showing one step of the manufacturing process of the present embodiment, respectively. In the laminating step STEP7, after the electrodes 150 are arranged in at least a part of the recesses 33 formed in the recess forming step STEP6, the first AlN calcined body 31 and the second AlN calcined body 32 are placed on the first flat surface. The 31a and the second flat surface 32a are laminated in contact with each other. As a result, the AlN sintered member 50 in which the electrode 150 is embedded becomes.

本発明のＡｌＮ焼結部材５０の製造方法においては、凹部を形成したＡｌＮ成形体同士を焼成して一体化する場合と比較して、凹部３３や電極１５０に由来するＡｌＮ焼結部材１０の各層の厚み、外形、中空構造がある場合の中空構造などの寸法精度の向上を図ることが可能となるため、例えば、絶縁層となる層の厚みのバラツキを所定の範囲に収まるように調整することもできる。その結果、例えば、電極埋設部材が静電チャックとして使用される場合、面内の吸着力の差を低減することができる。また、例えば、ヒーターとして用いられる場合、面内の温度のバラツキを低減することができる。 In the method for manufacturing the AlN sintered member 50 of the present invention, each layer of the AlN sintered member 10 derived from the recess 33 and the electrode 150 is compared with the case where the AlN molded bodies having the recesses formed are fired and integrated. Since it is possible to improve the dimensional accuracy of the thickness, outer shape, hollow structure, etc. when there is a hollow structure, for example, the variation in the thickness of the layer to be the insulating layer should be adjusted so as to be within a predetermined range. You can also. As a result, for example, when the electrode embedded member is used as an electrostatic chuck, the difference in suction force in the plane can be reduced. Further, for example, when used as a heater, it is possible to reduce in-plane temperature variation.

第１および第２のＡｌＮ脱脂体作製工程ＳＴＥＰ２では、以下の熱処理条件に従って脱脂することが好ましい。以下の熱処理条件に従って脱脂をする場合、第１および第２のＡｌＮ成形体形成工程ＳＴＥＰ１における第１または第２のＡｌＮ成形体１１、１２を形成するＡｌＮ原料粉は、少なくとも一方にＹ成分が添加されていることとする。添加されるＹ成分は、Ｙ２Ｏ３であることが好ましいが、脱脂時の熱処理によりＹ２Ｏ３となるものであってもよい。Ｙ成分は、ＡｌＮ原料粉に対し、Ｙ２Ｏ３に換算した内比で０．３～７．０ｗｔ％添加することが好ましい。バインダは、ＰＶＡ系であることが好ましい。 In the first and second AlN degreasing body manufacturing steps STEP2, it is preferable to degreasing according to the following heat treatment conditions. When degreasing is performed according to the following heat treatment conditions, the Y component is added to at least one of the AlN raw material powders forming the first or second AlN compacts 11 and 12 in the first and second AlN compact forming steps STEP1. It is assumed that it has been done. The Y component to be added is preferably Y 2 O 3 , but may be Y 2 O 3 by heat treatment during degreasing. The Y component is preferably added in an internal ratio of 0.3 to 7.0 wt% in terms of Y2O3 with respect to the AlN raw material powder. The binder is preferably PVA-based.

Ｙ成分が添加されるＡｌＮ原料粉は、第１のＡｌＮ成形体１１を形成するＡｌＮ原料粉および第２のＡｌＮ成形体１２を形成するＡｌＮ原料粉の両方であってもよい。両方に添加される場合、以下の熱処理条件は、両方に適用されることが好ましいが、一方のみに適用される場合も、本発明の方法に含む。また、以下の熱処理条件は、少なくとも電極１５０の上部に配置され、焼成後絶縁層となるＡｌＮ形成体に適用されることが好ましい。 The AlN raw material powder to which the Y component is added may be both the AlN raw material powder forming the first AlN molded body 11 and the AlN raw material powder forming the second AlN molded body 12. When added to both, the following heat treatment conditions are preferably applied to both, but cases to which only one is applied are also included in the method of the invention. Further, the following heat treatment conditions are preferably applied to an AlN forming body which is arranged at least above the electrode 150 and becomes an insulating layer after firing.

（熱処理条件）
Ｙ成分が添加された第１または第２のＡｌＮ成形体１１、１２は、脱脂温度Ｔ（℃）と脱脂時間Ｈ（ｈ）と添加したＹ成分をＹ２Ｏ３換算した内比でＣ（ｗｔ％）として、以下の式１および式２を満たすように制御して脱脂することで、第１または第２のＡｌＮ脱脂体２１、２２を作製することが好ましい。
Ｔ＞２０×Ｃ＋４４０ … （式１）
Ｈ≧３００／｛Ｔ－（２０×Ｃ＋４４０）｝ … （式２） (Heat treatment conditions)
In the first or second AlN molded bodies 11 and 12 to which the Y component was added, the degreasing temperature T (° C.), the degreasing time H (h), and the added Y component were converted into C (Y2O3). It is preferable that the first or second AlN degreasing bodies 21 and 22 are produced by controlling and degreasing so as to satisfy the following formulas 1 and 2 as wt%).
T> 20 × C + 440… (Equation 1)
H ≧ 300 / {T- (20 × C + 440)}… (Equation 2)

このような熱処理条件で作製された脱脂体を仮焼、焼成して作製されるセラミックス焼結体は、粒界にＹＡＧ粒子が含まれ、ＹＡＰ粒子およびＹＡＭ粒子が含まれなくなる。粒界にＹＡＧが生成するとＡｌＮセラミックスの体積抵抗率が相対的に低くなる。そのため、静電チャックの絶縁層として用いることに好適となる。本発明の１つの態様として静電チャックがあり、その静電吸着力は絶縁層の体積抵抗率に影響を受ける。絶縁層の体積抵抗率は、脱脂（熱処理）条件を上記の所定の条件することにより、ＡｌＮセラミックスの粒界にＹＡＧ組織のみを生成させることができる。ＹＡＧ組織のみが生成すると絶縁層の体積抵抗率は低くなる。 The ceramic sintered body produced by calcining and firing the degreased body produced under such heat treatment conditions contains YAG particles at the grain boundaries and does not contain YAP particles and YAM particles. When YAG is generated at the grain boundaries, the volume resistivity of AlN ceramics becomes relatively low. Therefore, it is suitable for use as an insulating layer of an electrostatic chuck. One embodiment of the present invention is an electrostatic chuck, and the electrostatic adsorption force thereof is affected by the volume resistivity of the insulating layer. As for the volume resistivity of the insulating layer, only the YAG structure can be generated at the grain boundaries of the AlN ceramics by subjecting the degreasing (heat treatment) conditions to the above-mentioned predetermined conditions. If only the YAG structure is generated, the volume resistivity of the insulating layer becomes low.

上記式はＹＡＧ組織のみが生成するときの脱脂（熱処理）条件式であり、焼結助剤の量Ｃの値によって図４のようにしきい式が表すグラフが変わってくる。すなわち、上記しきい式を充足する条件で脱脂したのちに仮焼体接合して静電チャックを作製すると絶縁層の厚みバラツキが抑えられ、かつ良好な静電吸着力を発揮させることができる。図４は、Ｙ成分の添加量としきい式の関係を例示した図である。 The above formula is a degreasing (heat treatment) condition formula when only the YAG structure is formed, and the graph represented by the threshold formula changes as shown in FIG. 4 depending on the value of the amount C of the sintering aid. That is, if an electrostatic chuck is manufactured by degreasing under the condition that the above-mentioned threshold is satisfied and then joining with a calcined body, the thickness variation of the insulating layer can be suppressed and a good electrostatic adsorption force can be exhibited. FIG. 4 is a diagram illustrating the relationship between the amount of the Y component added and the threshold formula.

（電極埋設部材の構成１）
次に、本実施形態に係る電極埋設部材の構成を説明する。図５は、本実施形態に係る電極埋設部材１００を示す正断面図である。電極埋設部材１００は、円板等の板状に形成され、絶縁層１１０、バルク層１２０および電極１５０を備える。絶縁層１１０およびバルク層１２０は、ＡｌＮを主成分とするセラミックス焼結体で形成されている。また、Ｙ２Ｏ３とＡｌ２Ｏ３の複酸化物の結晶相が含まれていてもよい。電極１５０には、モリブデンまたはタングステンが用いられる。図４に示す例では、電極１５０が、絶縁層１１０とバルク層１２０との間のみに設けられているが、電極が複数の層をなすように設けられていてもよい。その場合、処理対象を保持する側の最外層を絶縁層１１０、その他の層をバルク層１２０という。 (Structure of electrode embedded member 1)
Next, the configuration of the electrode embedded member according to the present embodiment will be described. FIG. 5 is a normal cross-sectional view showing the electrode embedded member 100 according to the present embodiment. The electrode burying member 100 is formed in a plate shape such as a disk, and includes an insulating layer 110, a bulk layer 120, and an electrode 150. The insulating layer 110 and the bulk layer 120 are formed of a ceramic sintered body containing AlN as a main component. Further, a crystal phase of a double oxide of Y 2 O 3 and Al 2 O 3 may be contained. Molybdenum or tungsten is used for the electrode 150. In the example shown in FIG. 4, the electrode 150 is provided only between the insulating layer 110 and the bulk layer 120, but the electrodes may be provided so as to form a plurality of layers. In that case, the outermost layer on the side holding the processing target is referred to as an insulating layer 110, and the other layers are referred to as a bulk layer 120.

絶縁層１１０の厚みのバラツキは、７５μｍ以下である。このように絶縁層１１０の厚みのバラツキが低減されていることにより、例えば、電極埋設部材１００が静電チャックとして使用される場合、面内の吸着力の差を低減することができる。また、例えば、ウエハ加熱用ヒーターとして用いられる場合、面内の温度のバラツキを低減することができる。 The variation in the thickness of the insulating layer 110 is 75 μm or less. By reducing the variation in the thickness of the insulating layer 110 in this way, for example, when the electrode embedded member 100 is used as an electrostatic chuck, it is possible to reduce the difference in the suction force in the plane. Further, for example, when it is used as a heater for heating a wafer, it is possible to reduce in-plane temperature variation.

絶縁層１１０を構成するセラミックス焼結体のＡｌＮ粒界には、ＹＡＧ粒子が含まれ、ＹＡＰ粒子およびＹＡＭ粒子が含まれないことが好ましい。これにより、絶縁層１１０の体積抵抗率を絶縁層１１０を構成するセラミックス焼結体のＡｌＮ粒界にＹＡＰ粒子またはＹＡＭ粒子が含まれ、ＹＡＧ粒子が含まれない場合と比べ相対的に低く調整することができ、例えば、電極埋設部材１００が静電チャックとして使用される場合、処理対象に対し強い静電吸着力を発揮できる。 It is preferable that the AlN grain boundaries of the ceramic sintered body constituting the insulating layer 110 contain YAG particles and do not contain YAP particles and YAM particles. As a result, the volume resistance of the insulating layer 110 is adjusted to be relatively low as compared with the case where the AlN grain boundaries of the ceramic sintered body constituting the insulating layer 110 contain YAP particles or YAM particles and do not contain YAG particles. For example, when the electrode-embedded member 100 is used as an electrostatic chuck, it can exert a strong electrostatic attraction force on a processing target.

なお、このような組成は、Ｘ線回折においてＹＡＧ、ＹＡＭ、ＹＡＰのピークが認められるか否かで評価できる。ピークか否かは、バックグラウンドの２倍以上の強度を示す先端があるか否かで判断できる。ＹＡＧ粒子が含まれるか否かは、ＪＣＰＤＳカードＩＣＤＤ＃０１－０７３－３１８４に示されたＹＡＧの回折ピークのうち、回折角度１８．１１°付近に表れるピークの有無で判断できる。ＹＡＭ粒子が含まれるか否かは、ＪＣＰＤＳカードＩＣＤＤ＃００－０３３－０３６８に示されたＹＡＭの回折ピークのうち、回折角度３０．６０°付近に表れるピークの有無で判断できる。ＹＡＰ粒子が含まれるか否かは、ＪＣＰＤＳカードＩＣＤＤ＃００－０３３－００４１に示されたＹＡＰの回折ピークのうち、回折角度３４．２４°付近に表れるピークの有無で判断できる。 It should be noted that such a composition can be evaluated by whether or not peaks of YAG, YAM, and YAP are observed in X-ray diffraction. Whether it is a peak or not can be determined by whether or not there is a tip showing an intensity twice or more that of the background. Whether or not YAG particles are contained can be determined by the presence or absence of a peak appearing near the diffraction angle 18.11 ° among the diffraction peaks of YAG shown in the JCPDS card ICDD # 01-073-3184. Whether or not YAM particles are contained can be determined by the presence or absence of a peak appearing near a diffraction angle of 30.60 ° among the diffraction peaks of YAM shown in the JCPDS card ICDD # 00-033-0368. Whether or not YAP particles are contained can be determined by the presence or absence of a peak appearing at a diffraction angle of 34.24 ° among the diffraction peaks of YAP shown in the JCPDS card ICDD # 00-033-0041.

バルク層１２０を構成するセラミックス焼結体のＡｌＮ粒界には、ＹＡＰ粒子またはＹＡＭ粒子が含まれ、ＹＡＧ粒子が含まれないことが好ましい。これにより、体積抵抗率を相対的に高く維持でき、リーク電流を抑止できる。なお、電極埋設部材１００は必ずしも静電チャックである必要はなく、電極１５０がヒーター用電極やＲＦ電源の電極として用いられてもよい。 It is preferable that the AlN grain boundaries of the ceramic sintered body constituting the bulk layer 120 contain YAP particles or YAM particles and do not contain YAG particles. As a result, the volume resistivity can be maintained relatively high, and the leakage current can be suppressed. The electrode embedded member 100 does not necessarily have to be an electrostatic chuck, and the electrode 150 may be used as a heater electrode or an RF power supply electrode.

（電極埋設部材の構成２）
図６は、電極埋設部材２００を示す正断面図である。電極埋設部材２００は、処理対象を表面上に保持する板状の保持部材２１０と、保持部材２１０の処理対象を保持する表面と対向する面に接合され、保持部材２１０を支持する支持部材２２０とを備えている。電極埋設部材２００は、例えば、ウエハ加熱用ヒーターや静電チャックとして用いることができる。なお、電極埋設部材２００も電極１５０がヒーター用電極やＲＦ電源の電極として用いられてもよい。 (Structure of electrode embedded member 2)
FIG. 6 is a normal cross-sectional view showing the electrode embedded member 200. The electrode-embedded member 200 includes a plate-shaped holding member 210 that holds the object to be processed on the surface, and a support member 220 that is joined to the surface of the holding member 210 that faces the surface that holds the object to be processed and supports the holding member 210. It is equipped with. The electrode embedded member 200 can be used, for example, as a wafer heating heater or an electrostatic chuck. As for the electrode burying member 200, the electrode 150 may be used as a heater electrode or an RF power supply electrode.

保持部材２１０は、円板等の板状に形成され、絶縁層１１０、バルク層１２０および電極１５０を備える。絶縁層１１０およびバルク層１２０は、ＡｌＮを主成分とするセラミックス焼結体で形成されている。また、Ｙ２Ｏ３とＡｌ２Ｏ３の複酸化物の結晶相が含まれていてもよい。図６に示す例では、電極１５０が、絶縁層１１０とバルク層１２０との間のみに設けられているが、電極が複数の層をなすように設けられていてもよい。電極１５０には、モリブデンまたはタングステンが用いられる。 The holding member 210 is formed in a plate shape such as a disk, and includes an insulating layer 110, a bulk layer 120, and an electrode 150. The insulating layer 110 and the bulk layer 120 are formed of a ceramic sintered body containing AlN as a main component. Further, a crystal phase of a double oxide of Y 2 O 3 and Al 2 O 3 may be contained. In the example shown in FIG. 6, the electrode 150 is provided only between the insulating layer 110 and the bulk layer 120, but the electrodes may be provided so as to form a plurality of layers. Molybdenum or tungsten is used for the electrode 150.

支持部材２２０は、円筒等の柱状に形成される。支持部材２２０は、ＡｌＮを主成分とするセラミック焼結体で形成されている。また、Ｙ２Ｏ３とＡｌ２Ｏ３の複酸化物の結晶相が含まれていてもよい。電極埋設部材２００が、ウエハ加熱用ヒーターとして用いられる場合、支持部材２２０は、熱伝導率を低くする観点から、Ｙ成分が含まれないことが好ましい。支持部材２２０は従前の接合材を用いた接合方法や接合材を用いない拡散接合によって一体化される。 The support member 220 is formed in a columnar shape such as a cylinder. The support member 220 is formed of a ceramic sintered body containing AlN as a main component. Further, a crystal phase of a double oxide of Y 2 O 3 and Al 2 O 3 may be contained. When the electrode-embedded member 200 is used as a wafer heating heater, it is preferable that the support member 220 does not contain the Y component from the viewpoint of lowering the thermal conductivity. The support member 220 is integrated by a conventional joining method using a joining material or diffusion joining without using a joining material.

なお、本発明は、上述した第１または第２の実施形態に具体的に記載したＡｌＮ焼結部材の製造方法、電極埋設部材の製造方法および電極埋設部材の構成に限定されるものではなく、特許請求の範囲に記載した範囲内であれば適宜変更することができる。例えば、ＡｌＮ焼結部材１０、５０は２個のＡｌＮ仮焼体が一体化したものであるが、３個以上のＡｌＮ仮焼体が一体化したものであってもよい。また、第２の実施形態において電極を埋設しない凹部が有っても、ＡｌＮセラミックスとしては一体化される。その場合、ＡｌＮ焼結部材に形成される中空構造はガス流路や熱電対などの配線用の空間として利用されてもよい。 The present invention is not limited to the method for manufacturing the AlN sintered member, the method for manufacturing the electrode-embedded member, and the configuration of the electrode-embedded member specifically described in the first or second embodiment described above. It can be changed as appropriate within the scope of the claims. For example, the AlN sintered members 10 and 50 are those in which two AlN calcined bodies are integrated, but three or more AlN calcined bodies may be integrated. Further, even if there is a recess in which the electrode is not embedded in the second embodiment, it is integrated as AlN ceramics. In that case, the hollow structure formed in the AlN sintered member may be used as a space for wiring such as a gas flow path and a thermocouple.

［実施例および比較例］
（試料ａ１～ａ２１、ｂ１～ｂ４）
図７および図８は各試料の製造条件および評価結果を示す表である。実施例ａ１～ａ２１、ｂ１～ｂ４は、まず、第１および第２のＡｌＮ成形体形成工程ＳＴＥＰ１として、純度９８％、平均粒径０．５μｍのＡｌＮ粉末に、焼結助剤としてＹ２Ｏ３を０．３～５質量％、成形助剤としてＰＶＡなどのバインダなどを添加したものを原料粉末とした。次に、この原料粉末をスプレードライヤーで顆粒化して顆粒を得た。 [Examples and Comparative Examples]
(Samples a1 to a21, b1 to b4)
7 and 8 are tables showing the production conditions and evaluation results of each sample. In Examples a1 to a21 and b1 to b4, first, as the first and second AlN molded body forming steps STEP1, AlN powder having a purity of 98% and an average particle size of 0.5 μm was added to Y2 O as a sintering aid. The raw material powder was prepared by adding 0.3 to 5% by mass of 3 and a binder such as PVA as a molding aid. Next, this raw material powder was granulated with a spray dryer to obtain granules.

そして、この顆粒を金型に充填し、圧力を２０ＭＰａとした一軸加圧成形して２個のＡｌＮ成形体を得た。 Then, the granules were filled in a mold and uniaxially pressure-molded at a pressure of 20 MPa to obtain two AlN molded articles.

次に、第１および第２のＡｌＮ脱脂体作製工程ＳＴＥＰ２として、これらＡｌＮ成形体を大気雰囲気炉内にて図７または図８の表に記載する熱処理条件で脱脂とともに熱処理を行い２個のＡｌＮ脱脂体を得た。 Next, as the first and second AlN degreasing body manufacturing steps STEP2, these AlN molded bodies are heat-treated together with degreasing under the heat treatment conditions shown in the table of FIG. 7 or FIG. 8 in an air atmosphere furnace to perform two AlNs. A degreased body was obtained.

次に、第１および第２のＡｌＮ仮焼体作製工程ＳＴＥＰ３として、これらＡｌＮ脱脂体を還元雰囲気炉内にて窒素雰囲気で炉内温度を実施例ａ１～ａ２１において１７００℃として３時間焼成、実施例ｂ１～ｂ４においては１１００～１８００℃、３時間として各水準２個のＡｌＮ仮焼体を得た。 Next, as the first and second AlN calcined body preparation steps STEP3, these AlN degreased bodies were fired in a reducing atmosphere furnace in a nitrogen atmosphere at a furnace temperature of 1700 ° C. for 3 hours. In Examples b1 to b4, two AlN calcined bodies of each level were obtained at 1100 to 1800 ° C. for 3 hours.

次に、第１および第２の平面形成工程ＳＴＥＰ４、５として、２個のＡｌＮ仮焼体に、第１および第２の平面を形成した。第１および第２の平面の算術平均粗さ（Ｒａ）および最大高さ（Ｒｚ）の平均は、Ｒａが０．２～０．６μｍ、Ｒｚが２～６μｍであった。 Next, as the first and second plane forming steps STEP4 and 5, the first and second planes were formed on the two AlN calcined bodies. The average arithmetic mean roughness (Ra) and maximum height (Rz) of the first and second planes was 0.2 to 0.6 μm for Ra and 2 to 6 μm for Rz.

次に、凹部形成工程ＳＴＥＰ６として、第２のＡｌＮ仮焼体の第２の平面に凹部を形成した。凹部は、深さ０．１ｍｍの円形状とした。 Next, as the recess forming step STEP6, a recess was formed on the second plane of the second AlN calcined body. The concave portion has a circular shape with a depth of 0.1 mm.

次に、積層工程ＳＴＥＰ７として、凹部に電極を配置して、第１のＡｌＮ仮焼体と第２のＡｌＮ仮焼体とを、電極を凹部に配置した後、第１の平面と第２の平面とを接触させた状態で積層させた。配置した電極の性状は以下の通りである。 Next, as the laminating step STEP7, an electrode is arranged in the recess, and the first AlN calcined body and the second AlN calcined body are arranged in the recess, and then the first plane and the second They were laminated in contact with a flat surface. The properties of the arranged electrodes are as follows.

（電極の性状）
材質：モリブデン
形態：メッシュ（平織り）、メッシュサイズ＃５０、モリブデンワイヤー径０．１ｍｍ (Properties of electrodes)
Material: Molybdenum Form: Mesh (plain weave), mesh size # 50, molybdenum wire diameter 0.1 mm

次に、焼成工程ＳＴＥＰ８として、このように積層した第１および第２のＡｌＮ仮焼体を焼成炉内にて窒素雰囲気で押圧板としてのカーボン平板で挟み込んで、１８００℃、１ＭＰａ、２時間、窒素雰囲気中で焼結して、試料ａ１～ａ２１、試料ｂ１～ｂ４を作製した。これにより、ＡｌＮ焼結部材（電極埋設部材）が得られた。 Next, as the firing step STEP8, the first and second AlN calcined bodies thus laminated were sandwiched between carbon flat plates as a pressing plate in a nitrogen atmosphere in a firing furnace, and the temperature was 1800 ° C., 1 MPa, 2 hours. Samples a1 to a21 and samples b1 to b4 were prepared by sintering in a nitrogen atmosphere. As a result, an AlN sintered member (electrode embedded member) was obtained.

（試料ｃ１～ｃ３）
また、比較例として、試料ｃ１～ｃ３を作製した。試料ｃ１およびｃ２は、いわゆる成形体ホットプレス法（特許６１４８８４５号公報に記載された方法）によって作製した。すなわち、実施例と同様に作製したＡｌＮ成形体に凹部加工を行った後、脱脂処理を行い、その後に電極を凹部に配置後、脱脂体を積層し、ホットプレス焼成（１８００℃、１ＭＰａ、２時間）した。試料ｃ１とｃ２は脱脂条件のみ異なり、ｃ１は脱脂温度６００℃、脱脂時間１２時間とし、ｃ２は脱脂温度６００℃、脱脂時間４時間とした。 (Samples c1 to c3)
Further, as a comparative example, samples c1 to c3 were prepared. The samples c1 and c2 were prepared by a so-called molded body hot press method (method described in Japanese Patent No. 6148845). That is, the AlN molded body produced in the same manner as in the examples was subjected to recess processing, followed by degreasing treatment, and then the electrodes were placed in the recesses, and then the degreased bodies were laminated and hot press fired (1800 ° C., 1 MPa, 2). Time). Samples c1 and c2 differed only in degreasing conditions. C1 had a degreasing temperature of 600 ° C. and a degreasing time of 12 hours, and c2 had a degreasing temperature of 600 ° C. and a degreasing time of 4 hours.

試料ｃ３は、いわゆる粉末ホットプレス法によって電極埋設部材を作製した。すなわち、ＡｌＮ粉末をカーボン型に充填後、電極を配置し、更にその上にＡｌＮ粉末を充填し、ホットプレス焼成（１８００℃、１ＭＰａ、２時間）した。なお、試料ｃ３の作製工程には、脱脂工程はない。 For sample c3, an electrode-embedded member was prepared by a so-called powder hot press method. That is, after filling the carbon mold with the AlN powder, an electrode was placed, the AlN powder was further filled therein, and hot press firing (1800 ° C., 1 MPa, 2 hours) was performed. There is no degreasing step in the step of preparing the sample c3.

（絶縁層の厚みのバラツキ評価）
そして、これらのＡｌＮ焼結部材の各試料に対して、絶縁層の厚みが平均で１ｍｍとなるように研削加工し、所定の位置の絶縁層の厚さを測定した。絶縁層の厚みは渦電流計で面内１７か所（中心、R70-8等配、R140-8等配）で測定し、平均値および最小値、最大値を記録した。 (Evaluation of variation in the thickness of the insulating layer)
Then, each sample of these AlN sintered members was ground so that the thickness of the insulating layer was 1 mm on average, and the thickness of the insulating layer at a predetermined position was measured. The thickness of the insulating layer was measured at 17 locations in the plane (center, R70-8 equal distribution, R140-8 equal distribution) with an eddy current meter, and the average value, minimum value, and maximum value were recorded.

結果は、本発明による試料ａ１～ａ２１の絶縁層のバラツキ（絶縁層厚み測定値の最大値－最小値）は３５～５８μｍであった。試料ｂ１は仮焼体の凹部形成工程で仮焼体の強度不足から破損し以後の工程は実施できなかった。試料ｂ２の絶縁層のバラツキは７５μｍ、試料ｂ３は、６０μｍであった。試料ｂ４は、焼成工程において第１の平面と第２の平面の間で接合不良が生じ評価ができなかった。また比較例として、従来の製法による試料ｃ１～ｃ３の絶縁層のバラツキは、ｃ１が９８μｍ、ｃ２が９５μｍ、ｃ３が２１０μｍであった。 As a result, the variation of the insulating layer of the samples a1 to a21 according to the present invention (maximum value-minimum value of the measured value of the insulating layer thickness) was 35 to 58 μm. Sample b1 was damaged in the process of forming the recesses of the calcined body due to insufficient strength of the calcined body, and the subsequent steps could not be carried out. The variation of the insulating layer of the sample b2 was 75 μm, and that of the sample b3 was 60 μm. Sample b4 could not be evaluated due to poor bonding between the first plane and the second plane in the firing step. As a comparative example, the variation of the insulating layers of the samples c1 to c3 by the conventional production method was 98 μm for c1, 95 μm for c2, and 210 μm for c3.

本発明の製法によって絶縁層のバラツキが従来製法によって作製された比較例と比較して改善されることが確認された。 It was confirmed that the variation of the insulating layer was improved by the production method of the present invention as compared with the comparative example produced by the conventional production method.

（体積抵抗率の測定）
次に、絶縁層の体積抵抗率を測定した。体積抵抗率の測定は、ＪＩＳ Ｃ２１３９に準拠する方法で測定した。セラミック焼結体の両面に耐熱金属（Ｎｉ）の電極を配置し、電極間に電圧（５００Ｖ）を印加し、電流を微小電流計（エーディーシー社Ｒ８３４０Ａ）で測定した。温度は、３００℃で測定した。そして、セラミック焼結体および電極寸法より体積抵抗率に換算した。体積抵抗率は、高圧電源と電流計により同様に電流値から算出してもよい。結果は、図７または図８の表に示す通りであった。 (Measurement of volume resistivity)
Next, the volume resistivity of the insulating layer was measured. The volume resistivity was measured by a method according to JIS C2139. Heat-resistant metal (Ni) electrodes were placed on both sides of the ceramic sintered body, a voltage (500 V) was applied between the electrodes, and the current was measured with a micro ammeter (ADC R8340A). The temperature was measured at 300 ° C. Then, it was converted into volume resistivity from the ceramic sintered body and the electrode dimensions. The volume resistivity may be similarly calculated from the current value by a high voltage power supply and an ammeter. The results were as shown in the table of FIG. 7 or FIG.

結果は、試料ａ１～ａ２１を参照し、焼結助剤としてＹ２Ｏ３を内比でＣ（ｗｔ％）添加して作製したＡｌＮ成形体を、脱脂温度Ｔ（℃）と脱脂時間Ｈ（ｈ）として、Ｔ＞２０×Ｃ＋４４０かつＨ≧３００／｛Ｔ－（２０×Ｃ＋４４０）｝の熱処理条件を施したものは体積抵抗率が低下し、静電チャックの絶縁層として機能することがわかった。 For the results, refer to the samples a1 to a21, and add Y2O3 as a sintering aid at an internal ratio of C (wt%) to the AlN molded product, which was prepared by adding a degreasing temperature T (° C.) and a degreasing time H ( ° C). As h), it was found that the one subjected to the heat treatment conditions of T> 20 × C + 440 and H ≧ 300 / {T- (20 × C + 440)} has a reduced volume resistivity and functions as an insulating layer of the electrostatic chuck. rice field.

（４点曲げ強度）
次に、特性評価後のＡｌＮ焼結体を切断し、４点曲げ強度試験を行った。その結果、試料ａ１～ａ２１の各々の１０点の測定値の平均値が、最小値２６０ＭＰａ、最大値３２０ＭＰａであり仮焼体接合後に得られるＡｌＮ焼結体部材として十分な機械的強度があることが確かめられた。 (4 point bending strength)
Next, the AlN sintered body after the characteristic evaluation was cut and a 4-point bending strength test was performed. As a result, the average value of the measured values at each of the 10 points of the samples a1 to a21 is 260 MPa at the minimum value and 320 MPa at the maximum value, and the AlN sintered body member obtained after the calcined body bonding has sufficient mechanical strength. Was confirmed.

（結晶相の確認）
次に、切断面を研磨加工した後、接合部および電極を拡大鏡などを用いて実験者が目視した。その結果、接合部に接合不良や破損などは確認されなかった。また、Ｘ線回折装置（Rigaku MultiFlex Cu Kα 40kV/40mA）を用いたＡｌＮ焼結体の粒界観察を行った。 (Confirmation of crystal phase)
Next, after the cut surface was polished, the experimenter visually inspected the joint and the electrode using a magnifying glass or the like. As a result, no joint failure or breakage was confirmed at the joint. In addition, the grain boundaries of the AlN sintered body were observed using an X-ray diffractometer (Rigaku MultiFlex Cu Kα 40kV / 40mA).

その結果、熱処理条件（脱脂条件）によって粒界に生成するイットリウム酸化物の結晶相が異なっていることが確認された。すなわち、粒界にＹＡＧ（Ｙ３Ａｌ５Ｏ１２）が生成し、ＹＡＰ（ＹＡｌＯ３）、ＹＡＭ（Ｙ４Ａｌ２Ｏ９）が生成していないものは３００℃での体積抵抗率が相対的に低くなっていることが確認された。また、ＹＡＧが生成せず、ＹＡＰやＹＡＭが生成しているものは相対的に体積抵抗率が高くなっていることが確認された。また、従来製法による比較例のうち、脱脂時間が短かった試料ｃ２の組織はＹＡＧ（Ｙ３Ａｌ５Ｏ１２）、ＹＡＭ（Ｙ４Ａｌ２Ｏ９）が生成しておらず、ＹＡＰ（ＹＡｌＯ３）が生成していた。また、脱脂工程を設けていない試料ｃ３の組織はＹＡＧ（Ｙ３Ａｌ５Ｏ１２）が生成しておらず、ＹＡＰ（ＹＡｌＯ３）、ＹＡＭ（Ｙ４Ａｌ２Ｏ９）が生成していた。なお、従来製法による比較例のうち、脱脂時間が長かった試料ｃ１は、ＹＡＧ（Ｙ３Ａｌ５Ｏ１２）が生成し、ＹＡＰ（ＹＡｌＯ３）、ＹＡＭ（Ｙ４Ａｌ２Ｏ９）が生成していなかった。 As a result, it was confirmed that the crystal phase of the yttrium oxide formed at the grain boundaries differs depending on the heat treatment conditions (defatting conditions). That is, those in which YAG (Y3 Al 5 O 12 ) is generated at the grain boundaries and YAP ( YAlO 3 ) and YAM (Y 4 Al 2 O 9 ) are not generated have a relative volume resistivity at 300 ° C. It was confirmed that it was low. Further, it was confirmed that those in which YAG was not generated and YAP and YAM were generated had a relatively high volume resistivity. Further, among the comparative examples by the conventional production method, YAG (Y 3 Al 5 O 12 ) and YAM (Y 4 Al 2 O 9 ) were not produced in the structure of the sample c2 whose degreasing time was short, and YAP (YAlO 3 ) was not produced. ) Was generated. Further, YAG (Y3 Al 5 O 12 ) was not produced in the structure of the sample c3 not provided with the degreasing step, and YAP ( YAlO 3 ) and YAM (Y 4 Al 2 O 9 ) were produced. Of the comparative examples produced by the conventional method, the sample c1 having a long degreasing time was produced by YAG (Y3 Al 5 O 12 ), and YAP ( YAlO 3 ) and YAM (Y 4 Al 2 O 9 ). I wasn't.

ＡｌＮセラミックスは本来体積抵抗率の高い絶縁体であるが、静電チャックの絶縁層として使用するには、ジョンセンラーベック力を誘起して強い静電吸着力を発現させるため絶縁層の体積抵抗率は一定程度低くすることが好ましい。そのため、ＹＡＧのみが生成しているＡｌＮセラミックス組織からなる実施例は、特に静電チャックとしての用途に好適であることが確かめられた。 AlN ceramics is originally an insulator with high volume resistivity, but when used as an insulating layer of an electrostatic chuck, the volume resistance of the insulating layer is to induce a Johnsen Labeck force to develop a strong electrostatic adsorption force. The rate is preferably lowered to a certain extent. Therefore, it was confirmed that the example consisting of an AlN ceramic structure in which only YAG is produced is particularly suitable for use as an electrostatic chuck.

なお、脱脂条件と体積抵抗率低下の関係については、脱脂によりＡｌＮ粒子の表面にＡｌ２Ｏ３のような酸化物が生成し、これと焼結助剤のＹ２Ｏ３が反応してイットリウムアルミニウム酸化物（ＹＡＧ、ＹＡＰ、ＹＡＭ）が生成する。このときＹ２Ｏ３の量に対してＡｌ２Ｏ３の量が多いとき、すなわち脱脂条件で温度が高くかつ脱脂時間が長い場合にＹＡＧが生成されると考えられる。 Regarding the relationship between the degreasing conditions and the decrease in volume resistance, degreasing produces oxides such as Al 2 O 3 on the surface of AlN particles, which react with the sintering aid Y 2 O 3 to yttrium. Aluminum oxides (YAG, YAP, YAM) are produced. At this time, it is considered that YAG is generated when the amount of Al 2 O 3 is larger than the amount of Y 2 O 3 , that is, when the temperature is high and the degreasing time is long under degreasing conditions.

図７または図８の表には、Ｙ２Ｏ３添加量、脱脂時間、および脱脂温度とＡｌＮ焼結体の粒界の生成粒子の結晶相を測定した結果をまとめた。これらを整理すると、脱脂温度Ｈ（℃）と脱脂時間、Ｙの添加量がＹ２Ｏ３換算でＣ（ｗｔ％）としてＴ＞２０×Ｃ＋４４０かつＨ≧３００／｛Ｔ－（２０×Ｃ＋４４０）｝であるときが粒界にＹＡＧが生成し静電チャックの絶縁層として更に好適であることが確認された。 The table of FIG. 7 or FIG. 8 summarizes the results of measuring the amount of Y2O3 added , the degreasing time , the degreasing temperature, and the crystal phase of the generated particles at the grain boundaries of the AlN sintered body. To summarize these, the degreasing temperature H (° C.), the degreasing time, and the amount of Y added are T> 20 × C + 440 and H ≧ 300 / {T- (20 × C + 440) as C (wt%) in terms of Y2O3. }, It was confirmed that YAG was generated at the grain boundaries and was more suitable as an insulating layer for the electrostatic chuck.

以上により、本発明のＡｌＮ焼結部材の製造方法は、寸法精度の向上したＡｌＮ焼結部材を製造できることが分かった。また、本発明のＡｌＮ焼結部材（電極埋設部材）の製造方法は、絶縁層の厚みのバラツキを低減でき、体積抵抗率を小さい範囲で制御できることが分かった。また、本発明の電極埋設部材は、静電チャックやウエハ加熱用ヒーターとして好適であることが確かめられた。 From the above, it was found that the method for manufacturing an AlN sintered member of the present invention can manufacture an AlN sintered member with improved dimensional accuracy. Further, it was found that the method for manufacturing an AlN sintered member (electrode embedded member) of the present invention can reduce the variation in the thickness of the insulating layer and control the volume resistivity within a small range. Further, it was confirmed that the electrode-embedded member of the present invention is suitable as an electrostatic chuck or a heater for heating a wafer.

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。 It goes without saying that the present invention is not limited to the above embodiments and extends to various modifications and equivalents included in the idea 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.

１０、５０ ＡｌＮ焼結部材
１１ 第１のＡｌＮ成形体
１２ 第２のＡｌＮ成形体
２１ 第１のＡｌＮ脱脂体
２２ 第２のＡｌＮ脱脂体
３１ 第１のＡｌＮ仮焼体
３１ａ 第１の平面
３２ 第２のＡｌＮ仮焼体
３２ａ 第２の平面
３３ 凹部
４１ 第１のＡｌＮ焼結体
４２ 第２のＡｌＮ焼結体
１００、２００ 電極埋設部材
１１０ 絶縁層
１２０ バルク層
１５０ 電極
２１０ 保持部材
２２０ 支持部材
10, 50 AlN sintered member 11 First AlN molded body 12 Second AlN molded body 21 First AlN degreased body 22 Second AlN degreased body 31 First AlN calcined body 31a First flat surface 32 First 2 AlN calcined body 32a Second flat surface 33 Recessed 41 First AlN sintered body 42 Second AlN sintered body 100, 200 Electrode embedded member 110 Insulation layer 120 Bulk layer 150 Electrode 210 Holding member 220 Support member

Claims (7)

ＡｌＮを主成分とするセラミックス焼結体で形成されたＡｌＮ焼結部材の製造方法であって、
ＡｌＮ原料粉から第１および第２のＡｌＮ成形体を形成する工程と、
前記第１および第２のＡｌＮ成形体を所定の温度以上、所定の時間以上脱脂処理して第１および第２のＡｌＮ脱脂体を作製する工程と、
前記第１および第２のＡｌＮ脱脂体を仮焼して第１および第２のＡｌＮ仮焼体を作製する工程と、
前記第１のＡｌＮ仮焼体に第１の平面を形成する工程と、
前記第２のＡｌＮ仮焼体に第２の平面を形成する工程と、
前記第１の平面または前記第２の平面の少なくとも一方に凹部を形成する工程と、
前記第１のＡｌＮ仮焼体と前記第２のＡｌＮ仮焼体とを、前記第１の平面と前記第２の平面とを接触させた状態で積層する工程と、
前記積層した前記第１のＡｌＮ仮焼体および前記第２のＡｌＮ仮焼体を、積層方向に１０ｋｇｆ／ｃｍ２以上の圧力を加えながら焼成する工程と、を備えることを特徴とするＡｌＮ焼結部材の製造方法。 A method for manufacturing an AlN sintered member formed of a ceramic sintered body containing AlN as a main component.
The process of forming the first and second AlN compacts from the AlN raw material powder, and
A step of degreasing the first and second AlN compacts at a predetermined temperature or higher and for a predetermined time or longer to prepare the first and second AlN degreased bodies.
The step of calcining the first and second AlN degreased bodies to prepare the first and second AlN calcined bodies, and
The step of forming the first plane on the first AlN calcined body and
The step of forming the second plane on the second AlN calcined body, and
The step of forming a recess in at least one of the first plane or the second plane, and
A step of laminating the first AlN calcined body and the second AlN calcined body in a state where the first plane and the second plane are in contact with each other.
AlN sintering comprising the step of firing the laminated first AlN calcined body and the second AlN calcined body while applying a pressure of 10 kgf / cm 2 or more in the laminating direction. Manufacturing method of parts. 前記第１および第２のＡｌＮ仮焼体を作製する工程の仮焼温度は、１２００℃以上１７００℃以下であり、かつ、前記焼成する工程の焼成温度は、１８００℃以上２０００℃以下であることを特徴とする請求項１記載のＡｌＮ焼結部材の製造方法。 The calcining temperature in the step of producing the first and second AlN calcined bodies is 1200 ° C. or higher and 1700 ° C. or lower, and the firing temperature in the firing step is 1800 ° C. or higher and 2000 ° C. or lower. The method for manufacturing an AlN sintered member according to claim 1, wherein the AlN sintered member is manufactured. 前記第１のＡｌＮ仮焼体と前記第２のＡｌＮ仮焼体とを積層する工程において、前記凹部の少なくとも一部に電極を配置して積層することを特徴とする請求項１または請求項２記載のＡｌＮ焼結部材の製造方法。 Claim 1 or claim 2 is characterized in that, in the step of laminating the first AlN calcined body and the second AlN calcined body, electrodes are arranged and laminated in at least a part of the recess. The method for manufacturing an AlN sintered member according to the description. 前記第１または第２のＡｌＮ成形体を形成する前記ＡｌＮ原料粉は、少なくとも一方にＹ成分が添加され、
前記第１および第２のＡｌＮ脱脂体を作製する工程において、Ｙ成分が添加された前記第１または第２のＡｌＮ成形体は、脱脂温度Ｔ（℃）と脱脂時間Ｈ（ｈ）と添加したＹ成分をＹ２Ｏ３換算した内比でＣ（ｗｔ％）として、Ｔ＞２０×Ｃ＋４４０かつＨ≧３００／｛Ｔ－（２０×Ｃ＋４４０）｝を満たす条件で前記第１または第２のＡｌＮ脱脂体が作製されることを特徴とする請求項３記載のＡｌＮ焼結部材の製造方法。 The AlN raw material powder forming the first or second AlN molded product has a Y component added to at least one of the powders.
In the step of producing the first and second AlN degreased bodies, the first or second AlN molded body to which the Y component was added was added with a degreasing temperature T (° C.) and a degreasing time H (h). The first or second AlN is satisfied under the condition that T> 20 × C + 440 and H ≧ 300 / {T- (20 × C + 440)}, where the Y component is C (wt%) in the internal ratio converted to Y 2 O 3 . The method for producing an AlN sintered member according to claim 3, wherein a degreased body is produced. 一体に形成され、処理対象を表面上に保持する電極埋設部材であって、
ＡｌＮを主成分とするセラミックス焼結体で形成された絶縁層およびバルク層と、
前記絶縁層とバルク層との間に設けられた電極と、を備え、
前記絶縁層の厚みのバラツキは７５μｍ以下であることを特徴とする電極埋設部材。 An electrode-embedded member that is integrally formed and holds the object to be treated on the surface.
An insulating layer and a bulk layer formed of a ceramic sintered body containing AlN as a main component, and
An electrode provided between the insulating layer and the bulk layer is provided.
An electrode-embedded member having a variation in the thickness of the insulating layer of 75 μm or less. 前記絶縁層は、前記セラミックス焼結体のＡｌＮ粒界にＹＡＧ粒子が含まれ、ＹＡＰ粒子およびＹＡＭ粒子が含まれないことを特徴とする請求項５記載の電極埋設部材。 The electrode-embedded member according to claim 5, wherein the insulating layer contains YAG particles in the AlN grain boundaries of the ceramic sintered body and does not contain YAP particles and YAM particles. 前記電極埋設部材は、さらに、前記処理対象を保持する表面と対向する面にＡｌＮを主成分とするセラミックス焼結体で形成された支持部材が接合されていることを特徴とする請求項５または請求項６に記載の電極埋設部材。
5. The electrode embedded member according to claim 6.
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