JP2011148687A - Ceramic joined body and method for production thereof - Google Patents
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- 239000000919 ceramic Substances 0.000 title claims abstract description 183
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 239000004020 conductor Substances 0.000 claims abstract description 111
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 29
- 230000003746 surface roughness Effects 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 14
- 238000007731 hot pressing Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 abstract 1
- 238000005304 joining Methods 0.000 description 24
- 238000005245 sintering Methods 0.000 description 22
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 16
- 239000011148 porous material Substances 0.000 description 16
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 13
- 239000000843 powder Substances 0.000 description 13
- 229910052581 Si3N4 Inorganic materials 0.000 description 11
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 11
- 239000010408 film Substances 0.000 description 9
- 238000010304 firing Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 238000012545 processing Methods 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 229910021332 silicide Inorganic materials 0.000 description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000007751 thermal spraying Methods 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910016006 MoSi Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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- Ceramic Products (AREA)
- Container, Conveyance, Adherence, Positioning, Of Wafer (AREA)
Abstract
Description
本発明は、セラミックス接合体に関する。本発明のセラミックス接合体は、特にセラミックスヒータ、静電チャックまたはサセプタ等に好適である。 The present invention relates to a ceramic joined body. The ceramic joined body of the present invention is particularly suitable for a ceramic heater, an electrostatic chuck, a susceptor or the like.
半導体製造工程では、シリコンウエハ上に集積回路を形成するために、成膜やエッチング処理が行われる。これらの工程では導体を内蔵したセラミックス部材がセラミックスヒータ、静電チャック、サセプタ等として用いられている。このようなセラミックス部材においては、セラミックス部材の薄型化が望まれている。例えば静電チャックでは、絶縁層を薄くすることにより、静電吸着力を高めることができる。また、プラズマ処理装置内で高周波電力を負荷した場合に、薄型であればインピーダンスが小さいので電力のロスが少なくなる。さらに、部材に放熱性が求められる場合には、薄型が有利である。 In the semiconductor manufacturing process, film formation and etching are performed to form an integrated circuit on a silicon wafer. In these processes, a ceramic member containing a conductor is used as a ceramic heater, an electrostatic chuck, a susceptor, or the like. In such a ceramic member, it is desired to reduce the thickness of the ceramic member. For example, in an electrostatic chuck, the electrostatic attractive force can be increased by thinning the insulating layer. In addition, when high frequency power is loaded in the plasma processing apparatus, the power loss is reduced because the impedance is small if it is thin. Further, when the member is required to have heat dissipation, a thin shape is advantageous.
このような薄型のセラミックス部材の例として、特許文献１には、窒化アルミニウムグリーンシートに、タングステンもしくはモリブデンを主成分とするペーストを塗布して、電極となる層を形成し、次いで、グリーンシートを積層圧着し、さらにそれを焼成して得た静電チャックが開示されている。 As an example of such a thin ceramic member, Patent Document 1 discloses that an aluminum nitride green sheet is coated with a paste containing tungsten or molybdenum as a main component to form a layer serving as an electrode. An electrostatic chuck obtained by laminating and then firing it is disclosed.
また、同文献には、原料粉末を型に充填して、一軸加圧処理を施して円盤状成形体を形成し、この円盤状成形体の上に、電極となる円形金属薄板を載置して、続いて原料粉末を円形金属薄板の上にさらに所定の厚さに充填して、再び加圧しながら、ホットプレス焼成を行い、焼結体として得た静電チャックが開示されている。 In the same document, a raw material powder is filled into a mold and subjected to uniaxial pressure treatment to form a disk-shaped formed body, and a circular metal thin plate serving as an electrode is placed on the disk-shaped formed body. Subsequently, an electrostatic chuck obtained by filling a raw material powder on a circular metal thin plate to a predetermined thickness and performing hot press firing while pressing again to obtain a sintered body is disclosed.
さらに、特許文献２には、窒化アルミニウム基板の片面に、スクリーン印刷法により単極型Ｗ電極を印刷し、その上に、ドクターブレード法により作製した接合材料グリーンシートを載せ、さらに窒化アルミニウム基板を載せて熱処理して得た静電チャックが開示されている。 Further, in Patent Document 2, a monopolar W electrode is printed on one side of an aluminum nitride substrate by a screen printing method, and a bonding material green sheet produced by a doctor blade method is placed thereon, and an aluminum nitride substrate is further mounted. An electrostatic chuck obtained by mounting and heat treatment is disclosed.
しかしながら、上記のような方法は、いずれも電極となる導体を精度良く埋設することができない場合がある。グリーンシートを積層圧着する方法では、特許文献１に記載されているように、グリーンシートの積層体が、焼成した際に必ずしも全体が均一に収縮するわけではないので電極に歪みが生じることが多かった。また、この方法では、成形性、焼結性を確保するために、バインダを添加して成形性を確保しているので、焼結し易くするために焼結助剤を多く添加しなければならず、セラミックス焼結体の純度や組成等に制約があった。そのため所望の特性を得ることができない場合があった。 However, in any of the above methods, there is a case where a conductor serving as an electrode cannot be embedded with high accuracy. In the method of laminating and pressure-bonding green sheets, as described in Patent Document 1, the green sheet laminate does not always shrink uniformly when fired, so the electrodes are often distorted. It was. In this method, in order to ensure moldability and sinterability, a binder is added to ensure moldability. Therefore, a large amount of sintering aid must be added to facilitate sintering. First, there were restrictions on the purity and composition of the ceramic sintered body. Therefore, there are cases where desired characteristics cannot be obtained.
また、円盤状成形体を用いた方法では、成形体が柔らかいため円形金属薄板が変形し易く、またその上に粉末を充填する際に粉末が回りこむ場合があり、精度良く導体を埋設できない場合があった。 In addition, in the method using a disk-shaped formed body, the circular metal thin plate is easily deformed because the formed body is soft, and the powder may wrap around when filling the powder on it, and the conductor cannot be embedded with high accuracy. was there.
特許文献２のような接合材料グリーンシートを用いる場合も、接合材料の純度や組成等に制約があり、所望の特性を得ることができないことがあった。 Even when a bonding material green sheet as in Patent Document 2 is used, there are cases where the purity and composition of the bonding material are limited and desired characteristics cannot be obtained.
本発明は、これらの問題に鑑みてなされたものであり、高精度に導体が内蔵された薄型のセラミックス部材を提供するものである。 The present invention has been made in view of these problems, and provides a thin ceramic member incorporating a conductor with high accuracy.
本発明のセラミックス接合体の製造方法は、これらの問題を解決するため、相対密度９９％以上の第１及び第２のセラミックス焼結体、並びに空隙を有する導体を用意する工程と、前記第１及び第２のセラミックス焼結体の間に前記導体を挟み込み、ホットプレスすることにより、少なくとも一方の前記セラミックス焼結体がクリープして、前記空隙が埋まり、他方の前記セラミックス焼結体と接合する工程と、を含み前記第１及び第２のセラミックス焼結体は互いに共通する成分を主成分とし、少なくとも一方の前記セラミックス焼結体の平均粒径は７μｍ以下であることを特徴とする。 In order to solve these problems, the method for producing a ceramic joined body of the present invention includes a step of preparing first and second ceramic sintered bodies having a relative density of 99% or more, and a conductor having voids, And the second ceramic sintered body is sandwiched between the ceramic sintered bodies and hot-pressed to creep at least one of the ceramic sintered bodies to fill the gap and join the other ceramic sintered body. The first and second ceramic sintered bodies are composed mainly of components common to each other, and at least one of the ceramic sintered bodies has an average particle size of 7 μm or less.
本発明では、セラミックス焼結体同士を接合材を介さずに導体を挟み込んで接合する。接合材を用いないので純度や組成の制約を少なくでき、所望の特性を有するセラミックス焼結体を用いることができる。また、本発明では、導体の形状精度がセラミックス焼結体の板厚の寸法精度に依存するので、予めセラミックス焼結体の板厚の寸法精度を高めておけば、高精度に導体を内蔵させることができる。さらに、薄型のセラミックス焼結体を用いれば、接合後に大幅な加工を施すことなく製品のセラミックス部材を容易に得ることができる。なお、空隙を有する導体とは、第１及び第２のセラミックス焼結体の間に導体を挟み込んだとき、導体が面状に亘って存在するのではなく、導体の間に空隙が存在して、第１及び第２のセラミックス焼結体との間に導体が存在しない領域があることを意味する。 In the present invention, the sintered ceramics are joined to each other by sandwiching a conductor without using a joining material. Since no bonding material is used, restrictions on purity and composition can be reduced, and a ceramic sintered body having desired characteristics can be used. In the present invention, since the shape accuracy of the conductor depends on the dimensional accuracy of the thickness of the ceramic sintered body, if the dimensional accuracy of the thickness of the ceramic sintered body is increased in advance, the conductor is incorporated with high accuracy. be able to. Furthermore, if a thin ceramic sintered body is used, a ceramic member of a product can be easily obtained without performing significant processing after joining. The conductor having a gap means that when the conductor is sandwiched between the first and second ceramic sintered bodies, the conductor does not exist over the surface, but there is a gap between the conductors. This means that there is a region where no conductor exists between the first and second ceramic sintered bodies.
本発明において、前記導体の厚さは０．１５ｍｍ以下であることが好ましい。これは、少なくとも一方のセラミックス焼結体がクリープし、導体の空隙を通じて、他方のセラミックス焼結体に接触し接合されることから、導体の厚さは制御されていることが好ましいからである。 In the present invention, the conductor preferably has a thickness of 0.15 mm or less. This is because the thickness of the conductor is preferably controlled because at least one of the ceramic sintered bodies creeps and contacts and is bonded to the other ceramic sintered body through the voids of the conductor.
また、本発明において、前記導体の空隙の幅は、前記導体の厚さの２〜２００倍であることが好ましい。これは、上記のように、少なくとも一方のセラミックス焼結体がクリープして導体の空隙を通じて他方のセラミックス焼結体に接触し接合されるように、導体の厚さに加えて導体の空隙の幅が制御されていることが好ましいからである。 In the present invention, the width of the gap of the conductor is preferably 2 to 200 times the thickness of the conductor. This is because, as described above, the width of the conductor gap in addition to the thickness of the conductor so that at least one ceramic sintered body creeps and contacts and is joined to the other ceramic sintered body through the conductor gap. This is because is preferably controlled.
また、本発明において、前記第１のセラミックス焼結体及び前記第２のセラミックス焼結体の接合面の表面粗さをＲａ０．１μｍ以下として、接合された前記第１のセラミックス焼結体と前記第２のセラミックス焼結体との接合界面における残気孔率が４０％以下となることが好ましい。この場合、内蔵された導体間に十分な絶縁を確保することができ、得られたセラミックス接合体により静電チャックを構成した場合、良好な性能を発揮することが可能となる。 Further, in the present invention, the first ceramic sintered body joined to the first ceramic sintered body and the second ceramic sintered body having a surface roughness Ra of 0.1 μm or less and the joined It is preferable that the residual porosity at the bonding interface with the second ceramic sintered body is 40% or less. In this case, sufficient insulation can be ensured between the built-in conductors, and when the electrostatic chuck is constituted by the obtained ceramic joined body, good performance can be exhibited.
また、第１のセラミックス焼結体及び第２のセラミックス焼結体の接合面の表面粗さをＲａ０．０５μｍ以下、接合された第１のセラミックス焼結体と第２のセラミックス焼結体との接合界面における残気孔率を８％以下とすることがより好ましい。この場合、母材内の任意の直線状における気孔の発生頻度と、接合界面上の残気孔の発生頻度について、気孔の並びに遜色のないセラミックス接合体を得ることができる。 Further, the surface roughness of the joining surface of the first ceramic sintered body and the second ceramic sintered body is Ra 0.05 μm or less, and the first ceramic sintered body and the second ceramic sintered body are joined. The residual porosity at the bonding interface is more preferably 8% or less. In this case, it is possible to obtain a ceramic joined body having no pores inferior with respect to the occurrence frequency of pores in an arbitrary straight line in the base material and the occurrence frequency of residual pores on the bonding interface.
本発明のセラミックス接合体は、互いに共通する成分を主成分とする第１のセラミックス焼結体と第２のセラミックス焼結体とが接合材を介さずに接合されたセラミックス接合体であって、前記第１及び第２のセラミックス焼結体の間には、空隙を有する導体が挟み込まれており、少なくとも一方の前記セラミックス焼結体がクリープして前記空隙が埋まることにより、他方の前記セラミックス焼結体と接合されたことを特徴とする。 The ceramic joined body of the present invention is a ceramic joined body in which the first ceramic sintered body and the second ceramic sintered body mainly composed of mutually common components are joined without using a joining material, A conductor having a gap is sandwiched between the first and second ceramic sintered bodies, and at least one of the ceramic sintered bodies creeps to fill the gap, so that the other ceramic sintered body is filled. It is characterized by being joined to a ligature.
本発明では、所望のセラミックス焼結体同士を接合材を介さずに接合できるので、セラミックスの純度や組成の制約を少なくでき、例えば、ヒータ、静電チャック、サセプタ等において、所望の特性を容易に得ることができる。 In the present invention, since desired ceramic sintered bodies can be bonded together without using a bonding material, restrictions on the purity and composition of ceramics can be reduced. For example, desired characteristics can be easily obtained in heaters, electrostatic chucks, susceptors, etc. Can get to.
また、本発明において、前記導体の厚さは、０．１５ｍｍ以下であることが好ましい。これは、上記のように、少なくとも一方のセラミックス焼結体がクリープし、導体の空隙を通じて、もう一方のセラミックス焼結体に接触し接合されることから、導体の厚さは制御されていることが好ましいからである。導体の厚さが大きいと、接合が不十分になり気密性に問題が生じる恐れがある。 Moreover, in this invention, it is preferable that the thickness of the said conductor is 0.15 mm or less. This is because the thickness of the conductor is controlled because, as described above, at least one ceramic sintered body creeps and contacts and is joined to the other ceramic sintered body through the gap of the conductor. Is preferable. If the thickness of the conductor is large, the bonding may be insufficient and there may be a problem in airtightness.
また、本発明において、前記導体は、発熱抵抗体、静電電極またはＲＦ電極であることが好ましい。導体を発熱抵抗体として用いたものはヒータを構成し、静電電極として用いたものは静電チャックを構成し、ＲＦ電極として用いたものはサセプタを構成する。いずれもシリコンウエハ等の基板の支持部材として用いられるものである。 In the present invention, the conductor is preferably a heating resistor, an electrostatic electrode, or an RF electrode. Those using a conductor as a heating resistor constitute a heater, those used as an electrostatic electrode constitute an electrostatic chuck, and those used as an RF electrode constitute a susceptor. Both are used as support members for substrates such as silicon wafers.
本発明の静電チャックは、接合面の表面粗さがＲａ０．１μｍ以下である前記第１のセラミックス焼結体と前記第２のセラミックス焼結体とが接合され、前記第１のセラミックス焼結体と前記第２のセラミックス焼結体との接合界面における残気孔率が４０％以下であり、前記導体を電極とする本発明のセラミックス接合体からなる。 In the electrostatic chuck according to the present invention, the first ceramic sintered body and the second ceramic sintered body having a surface roughness Ra of 0.1 μm or less are bonded to each other, and the first ceramic sintered body is bonded. The residual porosity of the bonding interface between the body and the second ceramic sintered body is 40% or less, and the ceramic joined body of the present invention using the conductor as an electrode.
本発明では、内蔵された導体からなる電極間に十分な絶縁を確保することができ、良好な性能を発揮することが可能となる。 In the present invention, sufficient insulation can be ensured between electrodes made of a built-in conductor, and good performance can be exhibited.
高精度に導体が内蔵された薄型のセラミックス部材を提供できる。 A thin ceramic member with a built-in conductor can be provided with high accuracy.
以下、図面を参照してより詳細に説明する。図１は、本発明のセラミックス接合体１０の製造方法を示した概略断面図である。はじめに、図１（ａ）で示したように第１のセラミックス焼結体１１と第２のセラミックス焼結体１２と導体１３とを用意する。 Hereinafter, it will be described in more detail with reference to the drawings. FIG. 1 is a schematic cross-sectional view showing a method for producing a ceramic joined body 10 of the present invention. First, as shown in FIG. 1A, a first ceramic sintered body 11, a second ceramic sintered body 12, and a conductor 13 are prepared.
第１及び第２のセラミックス焼結体１１，１２は、相対密度９９％以上であることが好ましい。相対密度が低く焼結が進んでいない焼結体では、接合の際の変形が大きくなるためである。また、第１及び第２のセラミックス焼結体１１，１２を加工した後に接合に供する場合、相対密度が低いと欠け等の加工不良が起きるためである。 It is preferable that the first and second ceramic sintered bodies 11 and 12 have a relative density of 99% or more. This is because, in a sintered body having a low relative density and in which sintering has not progressed, deformation during joining becomes large. In addition, when the first and second ceramic sintered bodies 11 and 12 are processed and then used for joining, if the relative density is low, processing defects such as chipping occur.
セラミックス焼結体１１，１２の材料としては、アルミナ、マグネシア、スピネル、イットリア、ジルコニア等の酸化物の他、炭化珪素、窒化珪素、窒化アルミニウム等種々の材料を用いることができる。なかでも、酸化アルミニウム、窒化珪素、窒化アルミニウムを好適に用いることができる。各セラミックスの純度は、要求される特性に応じて定められる。例えば、使用温度において熱伝導率５０Ｗ／ｍＫ以上を要求される場合は窒化アルミニウムを用いることが好ましい。 As materials for the ceramic sintered bodies 11 and 12, various materials such as silicon carbide, silicon nitride, and aluminum nitride can be used in addition to oxides such as alumina, magnesia, spinel, yttria, and zirconia. Among these, aluminum oxide, silicon nitride, and aluminum nitride can be preferably used. The purity of each ceramic is determined according to the required characteristics. For example, aluminum nitride is preferably used when a thermal conductivity of 50 W / mK or more is required at the operating temperature.
これらの材料に副成分を加えても良い。副成分としては、焼結助剤の他、抵抗や色調を調整したり、強度を高めたりするための添加剤が挙げられる。これらは、１０質量％未満の含有量とすることが好ましい。副成分が多く含まれると、粒成長を調整することが困難になり、変形が大きくなったり、接合できなくなったりするためである。したがって、主成分は９０質量％以上含まれることが好ましい。 Subcomponents may be added to these materials. Examples of the auxiliary component include additives for adjusting resistance and color tone and increasing strength in addition to the sintering aid. It is preferable to make these content less than 10 mass%. This is because when a large amount of subcomponents are contained, it becomes difficult to adjust the grain growth, and deformation becomes large or bonding becomes impossible. Therefore, it is preferable that 90 mass% or more of a main component is contained.
焼結助剤としては、主成分が酸化アルミニウムの場合は、例えば酸化マグネシウム、酸化カルシウム、酸化ケイ素等であり、また遷移金属酸化物、希土類酸化物も含まれる場合がある。主成分が窒化アルミニウムの場合は、例えば酸化イットリウム等の希土類元素酸化物、酸化カルシウム等が用いられる。主成分が窒化珪素の場合は、例えば酸化イットリウム、酸化アルミニウム、酸化マグネシウム等を用いることができる。 As the sintering aid, when the main component is aluminum oxide, for example, magnesium oxide, calcium oxide, silicon oxide and the like may be included, and transition metal oxides and rare earth oxides may also be included. When the main component is aluminum nitride, for example, a rare earth element oxide such as yttrium oxide, calcium oxide, or the like is used. When the main component is silicon nitride, for example, yttrium oxide, aluminum oxide, magnesium oxide, or the like can be used.
また、第１と第２のセラミックス焼結体１１，１２の主成分は、同じものであることが好ましい。上記のように焼結助剤や添加剤等の副成分を含んでも良いが、主成分が異なる場合は、加熱及び冷却時の膨張及び収縮挙動のズレが大きくなるため、接合できなるおそれがある。 The main components of the first and second ceramic sintered bodies 11 and 12 are preferably the same. Subcomponents such as sintering aids and additives may be included as described above, but if the main components are different, there is a risk of expansion and contraction behavior during heating and cooling, which may result in bonding. .
セラミックス焼結体１１，１２の焼結は、常圧焼結、加圧焼結、ホットプレス焼結、反応焼結等種々の方法により行うことができる。本発明では、焼結と接合とを別々に行うので、セラミックス焼結体１１，１２に求められる特性を得るのに最適な焼結方法を採用できる。例えば、ホットプレス焼結では、脱脂不良が起きたり、色ムラが生じたりする場合があるが、これらの問題が生じ難いホットプレス焼結以外の常圧焼結等でセラミックス焼結体１１，１２を作製し、その後にホットプレス接合を行うことにより脱脂不良や色ムラが生じることなく導体１３が挟み込まれたセラミックス接合体１０を得ることができる。 The ceramic sintered bodies 11 and 12 can be sintered by various methods such as normal pressure sintering, pressure sintering, hot press sintering, and reactive sintering. In the present invention, since sintering and joining are performed separately, an optimum sintering method can be employed to obtain the characteristics required for the ceramic sintered bodies 11 and 12. For example, in hot press sintering, degreasing defects may occur or color unevenness may occur, but these problems are unlikely to occur, and ceramic sintered bodies 11 and 12 may be used in normal pressure sintering other than hot press sintering. Can be obtained, and then hot press bonding can be performed to obtain the ceramic bonded body 10 in which the conductor 13 is sandwiched without causing degreasing defects or color unevenness.
セラミックス焼結体１１，１２は、板状であり、一定の板厚を有することが望ましい。ホットプレスを用いて接合するため、板厚にばらつきがあると、局所的に負荷がかかり、変形や割れが生じるためである。具体的には、板厚のばらつきは、５μｍ以下とすることが好ましく、１μｍ以下とすることがより好ましい。板厚のばらつきは、電気マイクロメータを用いて任意１０箇所の板厚を測定し、その最大板厚と最小板厚の差により求めることができる。 The ceramic sintered bodies 11 and 12 are plate-shaped and desirably have a certain plate thickness. This is because, since bonding is performed using a hot press, if the plate thickness varies, a load is locally applied, and deformation and cracking occur. Specifically, the variation in the plate thickness is preferably 5 μm or less, and more preferably 1 μm or less. The variation in the plate thickness can be obtained by measuring the plate thickness at any 10 locations using an electric micrometer and calculating the difference between the maximum plate thickness and the minimum plate thickness.
本発明では、薄型のセラミックス焼結体１１，１２を接合に用いることができるので、接合後に大幅な加工を施すことなく製品のセラミックス部材１３を容易に得ることができる。従来のホットプレス焼結により導体を内蔵する方法では、導体の形状精度が悪かったため、それに合わせて加工代を確保するために、セラミックス焼結体の厚さを大きくしなければならなかったが、本発明では、接合前後での変形が小さいので、予め薄型のセラミックス焼結体１１，１２を用いることができる。したがって、製造コストを抑えつつ導体１３を内蔵した薄型のセラミックス接合体１０を容易に得ることができる。 In the present invention, since the thin ceramic sintered bodies 11 and 12 can be used for joining, the ceramic member 13 of the product can be easily obtained without performing significant processing after joining. In the conventional method of incorporating a conductor by hot press sintering, the shape accuracy of the conductor was poor, so the ceramic sintered body had to be increased in thickness in order to secure a processing allowance accordingly, In the present invention, since the deformation before and after joining is small, thin ceramic sintered bodies 11 and 12 can be used in advance. Therefore, it is possible to easily obtain a thin ceramic joined body 10 incorporating the conductor 13 while suppressing the manufacturing cost.
また、セラミックス焼結体１１，１２において導体１３を挟み込む側の面、すなわち接合面については表面粗さを調整しておくことが好ましい。表面粗さのばらつきが大きいと、クリープが起きるときや、セラミックス焼結体１１，１２同士がクリープにより接触し接合されるときにムラが生じ易いため、接合不良が発生する恐れがある。また、表面粗さをある程度小さくしておくことは導体１３の寸法精度を高めるためにも好ましい。セラミックス焼結体１１，１２の接合面の表面粗さＲｚ（ＪＩＳＢ０６０１−２００１）が、平均粒径の１／２以下とすること、または表面粗さＲａ（ＪＩＳＢ０６０１−２００１）が、０．２μｍ以下とすることが好ましい。 Further, it is preferable to adjust the surface roughness of the ceramic sintered bodies 11 and 12 on the side where the conductor 13 is sandwiched, that is, the bonding surface. If the variation in the surface roughness is large, unevenness is likely to occur when creep occurs or when the ceramic sintered bodies 11 and 12 are brought into contact with each other and joined together by creep. It is also preferable to reduce the surface roughness to some extent in order to increase the dimensional accuracy of the conductor 13. The surface roughness Rz (JISB0601-2001) of the joint surface of the ceramic sintered bodies 11 and 12 is set to 1/2 or less of the average particle diameter, or the surface roughness Ra (JISB0601-2001) is 0.2 μm or less. It is preferable that
なお、少なくとも一方のセラミックス焼結体１１，１２には、相対密度９９％以上を満たす範囲でボイドが含まれていても良い。ただし、ボイド径は、１０μｍ以下であることが好ましい。このようなボイドは、セラミックス焼結体１１，１２のクリープを促進するためである。 Note that at least one of the ceramic sintered bodies 11 and 12 may contain voids in a range satisfying a relative density of 99% or more. However, the void diameter is preferably 10 μm or less. This is because the voids promote the creep of the ceramic sintered bodies 11 and 12.
導体１３としては、箔、板、線、メッシュまたは繊維状のモリブデンやタングステン、白金、レニウム、クロム等の耐熱金属を用いることができる。これらを第１または第２のセラミックス焼結体１１，１２に真空蒸着法、スパッタリング法、イオンプレーティング法、ＰＶＤ法、ＣＶＤ法、溶射法等の成膜方法を用いて導体１３を形成してもよい。また、導体１３としてＴｉＣ、ＷＣ、ＳｉＣなどの金属炭化物、ＴｉＮ、ＣｒＮ、ＺｒＮ、などの金属窒化物やＭｏＳｉ２、ＶＳｉ２などの金属珪化物等の導電性セラミックスを用いてもよい。これらも同様に真空蒸着法、スパッタリング法、イオンプレーティング法、ＰＶＤ法、ＣＶＤ法、溶射法等の成膜方法を用いることにより、第１または第２のセラミックス焼結体１１，１２に形成することができる。導体１３は、発熱抵抗体、静電電極、またはＲＦ電極として機能する。 As the conductor 13, a heat-resistant metal such as foil, plate, wire, mesh, or fibrous molybdenum, tungsten, platinum, rhenium, or chromium can be used. The conductor 13 is formed on the first or second ceramic sintered bodies 11 and 12 by using a film forming method such as a vacuum evaporation method, a sputtering method, an ion plating method, a PVD method, a CVD method, or a thermal spraying method. Also good. The conductor 13 may be made of a metal carbide such as TiC, WC or SiC, a metal nitride such as TiN, CrN or ZrN, or a conductive ceramic such as a metal silicide such as MoSi 2 or VSi 2 . These are similarly formed on the first or second ceramic sintered bodies 11 and 12 by using a film forming method such as a vacuum deposition method, a sputtering method, an ion plating method, a PVD method, a CVD method, or a thermal spraying method. be able to. The conductor 13 functions as a heating resistor, an electrostatic electrode, or an RF electrode.
導体１３の厚さは、０．１５ｍｍ以下とすることが好ましい。セラミックス焼結体１１，１２の板厚のばらつきを小さくし、さらに導体１３の厚さを上記範囲とすることで、クリープによる接合が容易になる。導体１３の厚さのより好ましい範囲は、７０μｍ以下である。 The thickness of the conductor 13 is preferably 0.15 mm or less. By reducing the variation in the plate thickness of the ceramic sintered bodies 11 and 12 and further setting the thickness of the conductor 13 within the above range, joining by creep is facilitated. A more preferable range of the thickness of the conductor 13 is 70 μm or less.
導体１３が箔や板の場合には、セラミックス焼結体１１，１２同士の密着を確保するため、中抜き加工、スリット加工を施し、電極面積に対する空隙の面積比率を５〜９０％とすることが望ましい。導体１３がメッシュの場合には、＃６０メッシュ以上が望ましく、開口率３０％以上であることが望ましい。導体１３が線や繊維の場合には、線径０．１ｍｍ以下が望ましい。 In the case where the conductor 13 is a foil or a plate, in order to ensure the close contact between the ceramic sintered bodies 11 and 12, a hollowing process and a slitting process are performed, and the area ratio of the gap to the electrode area is 5 to 90%. Is desirable. When the conductor 13 is a mesh, # 60 mesh or more is desirable, and an aperture ratio of 30% or more is desirable. When the conductor 13 is a wire or a fiber, a wire diameter of 0.1 mm or less is desirable.
導体１３の空隙の幅は、導体１３の厚さの２〜２００倍とすることが好ましく、１５〜７５倍とすることがより好ましい。導体１３の空隙の幅は、空隙をセラミックス焼結体１１，１２の接合面に投射した平面で見たときの内接円の直径を用いる。したがって、例えば、空隙が長方形であれば、空隙の幅は短辺に等しくなる。空隙の幅が、導体１３の厚さに対して所定の範囲であれば、クリープによる接合が可能になり、少なくとも気密性を有するセラミックス接合体を得ることができる。なお、導体１３の外周端部からセラミックス焼結体１１，１２の外周端部までの距離も同様に導体１３の厚さの１０〜２００倍とすることが好ましく、１５〜７５倍とすることがより好ましい。 The width of the gap of the conductor 13 is preferably 2 to 200 times the thickness of the conductor 13, and more preferably 15 to 75 times. As the width of the gap of the conductor 13, the diameter of the inscribed circle when the gap is viewed on a plane projected onto the joint surface of the ceramic sintered bodies 11 and 12 is used. Thus, for example, if the gap is rectangular, the width of the gap is equal to the short side. If the width of the air gap is within a predetermined range with respect to the thickness of the conductor 13, joining by creep becomes possible, and at least a ceramic joined body having airtightness can be obtained. The distance from the outer peripheral end of the conductor 13 to the outer peripheral end of the ceramic sintered bodies 11 and 12 is preferably 10 to 200 times the thickness of the conductor 13 and preferably 15 to 75 times. More preferred.
次に、図１（ｂ）に示したように、第１及び第２のセラミックス焼結体１１，１２の間に導体１３を挟み込む。 Next, as illustrated in FIG. 1B, the conductor 13 is sandwiched between the first and second ceramic sintered bodies 11 and 12.
しかる後に、図１（ｃ）に示したように、ホットプレス接合する。ホットプレスにより、セラミックス焼結体１１に符号１１１で示したように、クリープが生じ、空隙を埋めて接合が可能となる。 Thereafter, hot press bonding is performed as shown in FIG. As indicated by reference numeral 111, the ceramic sintered body 11 is creeped by hot pressing, and the gap can be filled and bonding can be performed.
ホットプレスの雰囲気は、Ｎ２とした。導体１３が酸化や腐食しない不活性雰囲気であればよい。また、セラミックス焼結体１１，１２に耐酸化性がありかつ導体１３が白金や金属珪化物のような大気に対する耐酸化性が高いものなどである場合には、耐酸化性が得られる温度範囲内で大気雰囲気下でホットプレスすることが可能である。 Atmosphere of hot press was set to N 2. What is necessary is just the inert atmosphere which the conductor 13 does not oxidize or corrode. Moreover, when the ceramic sintered bodies 11 and 12 have oxidation resistance and the conductor 13 has high oxidation resistance to the atmosphere such as platinum or metal silicide, the temperature range in which oxidation resistance can be obtained. It is possible to hot press in an air atmosphere.
ホットプレスの圧力は、０．０１ＭＰａ〜２０ＭＰａの範囲が望ましい。 The pressure of the hot press is desirably in the range of 0.01 MPa to 20 MPa.
クリープにより接合させるには、雰囲気、プレス圧の制御に加えて、加熱温度を調整する必要があるが、加熱温度は、セラミックス焼結体１１，１２の焼結温度との関係で調整することが好ましい。 In order to join by creep, it is necessary to adjust the heating temperature in addition to the control of the atmosphere and the press pressure, but the heating temperature can be adjusted in relation to the sintering temperature of the ceramic sintered bodies 11 and 12. preferable.
ホットプレスの加熱温度は、特に限定されないが、少なくとも一方のセラミックス焼結体１１，１２の焼結温度よりも低いことが好ましい。少なくとも一方のセラミックス焼結体１１，１２の焼結温度よりも低い温度でホットプレスすれば、セラミックス焼結体１１，１２の粒成長を伴う変形が抑えられ、導体１３の形状精度を高めることができる。 The heating temperature of the hot press is not particularly limited, but is preferably lower than the sintering temperature of at least one of the ceramic sintered bodies 11 and 12. If hot pressing is performed at a temperature lower than the sintering temperature of at least one ceramic sintered body 11, 12, deformation accompanied by grain growth of the ceramic sintered body 11, 12 can be suppressed, and the shape accuracy of the conductor 13 can be improved. it can.
例えば、ホットプレスの加熱温度が第１のセラミックス焼結体１１の焼結温度よりも高く、第２のセラミックス焼結体１２の焼結温度よりも低い場合には、第１のセラミックス焼結体１１のクリープにより導体１３の空隙が埋められて接合が可能となる。このとき、第２のセラミックス焼結体１２は、接合前後で平均粒径の変化がなく、クリープによる変形がないことから導体１３もそれに倣って高精度に挟み込むことが可能となる。なお、本発明は、双方のセラミックス焼結体１１，１２の焼結温度よりも高温でホットプレスすることも可能であり、必ずしもそれを排除するものではない。 For example, when the heating temperature of the hot press is higher than the sintering temperature of the first ceramic sintered body 11 and lower than the sintering temperature of the second ceramic sintered body 12, the first ceramic sintered body 11, the gap of the conductor 13 is filled by the creep of 11 and the joining becomes possible. At this time, since the second ceramic sintered body 12 does not change in average particle diameter before and after joining and is not deformed by creep, the conductor 13 can also be sandwiched with high accuracy following that. In the present invention, hot pressing can be performed at a temperature higher than the sintering temperature of both ceramic sintered bodies 11 and 12, and this is not necessarily excluded.
さらに、ホットプレスによるクリープで接合するには、少なくとも一方のセラミックス焼結体の平均粒径を７μｍ以下、より好ましくは５μｍ以下、さらに好ましくは、４μｍ以下とすると良い。第１及び第２のセラミックス焼結体１１，１２のうち、少なくとも一方のセラミックス焼結体の平均粒径を上記のように制御することにより、導体１３を高精度に挟み込んだセラミックス接合体１０を得ることができる。 Furthermore, for joining by creep by hot pressing, the average particle size of at least one of the ceramic sintered bodies is 7 μm or less, more preferably 5 μm or less, and even more preferably 4 μm or less. By controlling the average particle size of at least one of the first and second ceramic sintered bodies 11 and 12 as described above, the ceramic joined body 10 sandwiching the conductor 13 with high accuracy is obtained. Obtainable.
例えば、第１のセラミックス焼結体１１の平均粒径が、第２のセラミックス焼結体１２の平均粒径よりも小さく７μｍ以下である場合には、第１のセラミックス焼結体１１がよりクリープし易いので、ホットプレスの加熱温度を調整することにより、第１のセラミックス焼結体１１のクリープにより、導体１３の空隙が埋められて接合が可能となる。このとき、平均粒径の大きい第２のセラミックス焼結体１２の粒成長が抑えられているのでクリープによる変形が少ないことから、導体１３もそれに倣って高精度に挟み込むことが可能となる。 For example, when the average particle diameter of the first ceramic sintered body 11 is smaller than the average particle diameter of the second ceramic sintered body 12 and is 7 μm or less, the first ceramic sintered body 11 is more creeped. Therefore, by adjusting the heating temperature of the hot press, the gap of the conductor 13 is filled by the creep of the first ceramic sintered body 11, and bonding becomes possible. At this time, since the grain growth of the second ceramic sintered body 12 having a large average particle diameter is suppressed and deformation due to creep is small, the conductor 13 can also be sandwiched with high accuracy following that.
また、セラミックス接合体１０の内部や表面に溝を形成したい場合には、ホットプレス接合のときにクリープによる変形のないセラミックス焼結体１１，１２に溝を形成することで、その形状精度を高めることができる。なお、本発明は、双方のセラミックス焼結体１１，１２の平均粒径を上記範囲としても接合することは可能であり、必ずしもそれを排除するものではない。 Further, when it is desired to form a groove in the ceramic bonded body 10 or on the surface, the groove is formed in the ceramic sintered bodies 11 and 12 which are not deformed by creep during hot press bonding, thereby improving the shape accuracy. be able to. In the present invention, it is possible to join even if the average particle diameter of the ceramic sintered bodies 11 and 12 is within the above range, and this is not necessarily excluded.
少なくとも一方のセラミックス焼結体１１，１２において、接合後の平均粒径と接合前の平均粒径と比べた粒成長率が、５０％以下であることが好ましい。本発明は、セラミックス焼結体１１，１２の粒成長を伴うクリープによりセラミックス焼結体同士を接合するものであるが、粒成長が大き過ぎると、変形が大きくなり導体の形状精度が低下するので好ましくない。なお、粒成長率は、接合後の平均粒径から接合前の平均粒径を引いた差を接合前の平均粒径で除した値を百分率で表したものである。 In at least one of the ceramic sintered bodies 11 and 12, it is preferable that the grain growth rate compared with the average particle diameter after bonding and the average particle diameter before bonding is 50% or less. In the present invention, the sintered ceramic bodies 11 and 12 are joined together by creep accompanied by grain growth of the ceramic sintered bodies 11 and 12, but if the grain growth is too large, deformation becomes large and the shape accuracy of the conductor is lowered. It is not preferable. The grain growth rate is a percentage obtained by dividing the difference obtained by subtracting the average particle size before bonding from the average particle size after bonding by the average particle size before bonding.
上記のような製法により、セラミックス接合体１０が得られる。本発明では、薄型のセラミックス焼結体１１，１２を用いれば、接合後に大幅な加工を施すことなく製品のセラミックス部材１０を容易に得ることができる。本発明では、例えば、接合後に加工を施すことなく、セラミックス接合体１０の総厚みを２ｍｍ以下とすることができる。また、接合後の加工を加えた場合には、例えば、セラミックス接合体１０の総厚みを１ｍｍ以下とすることができ、また、一方のセラミックス焼結体１１，１２の厚みを０．０５〜０．３ｍｍとすることができる。このように、本発明は、導体１３を内蔵した薄型のセラミックス接合体１０を得るのに適している。 The ceramic joined body 10 is obtained by the manufacturing method as described above. In the present invention, if the thin ceramic sintered bodies 11 and 12 are used, the product ceramic member 10 can be easily obtained without significant processing after joining. In the present invention, for example, the total thickness of the ceramic joined body 10 can be 2 mm or less without performing processing after joining. Moreover, when the process after joining is added, the total thickness of the ceramic joined body 10 can be made into 1 mm or less, for example, and the thickness of one ceramic sintered compact 11 and 12 is 0.05-0. .3 mm. Thus, the present invention is suitable for obtaining a thin ceramic joined body 10 incorporating the conductor 13.
なお、セラミックス接合体１０により静電チャックを構成する場合、内蔵された導体１３からなる電極間で導通がおこらないように、電極間の耐電圧γを充分に確保して絶縁する必要がある。しかしながら、セラミックス接合体１０は、接合界面に気孔が残存することがあり、それによる静電チャックの電極間の耐電圧γが低下するおそれがある。 When an electrostatic chuck is constituted by the ceramic bonded body 10, it is necessary to ensure insulation with a sufficient withstand voltage γ between the electrodes so that conduction does not occur between the electrodes composed of the built-in conductor 13. However, in the ceramic joined body 10, pores may remain at the joining interface, which may reduce the withstand voltage γ between the electrodes of the electrostatic chuck.
電極間の耐電圧γを高めるためには、図２を参照して、接合された第１及び第２のセラミックス焼結体１１，１２間の接合界面１４における残気孔（残存する空隙）１５を低減する必要がある。接合された部分と残気孔１５の部分との割合は残気孔率αで表され、接合界面１４における残気孔率αは４０％以下、より好ましくは８％以下である必要がある。 In order to increase the withstand voltage γ between the electrodes, referring to FIG. 2, residual pores (remaining voids) 15 at the bonding interface 14 between the bonded first and second ceramic sintered bodies 11 and 12 are formed. There is a need to reduce. The ratio between the joined portion and the residual pore 15 portion is represented by the residual porosity α, and the residual porosity α at the joint interface 14 needs to be 40% or less, more preferably 8% or less.
なお、残気孔率αを数値化する方法として、接合界面１４の撮影写真に基づいて求めることができる。図２に模式的に示すように、接合界面１４の長さをＬとして、各残気孔１５の接合界面１４上における長さａｉ、その合計長さをΣａｉとして、式（１）より残気孔率α（％）を、式（２）により接合率β（％）を算出することができる。 As a method for quantifying the residual porosity α, it can be obtained based on a photograph of the bonding interface 14. As schematically shown in FIG. 2, the length of the bonding interface 14 is L, the length ai of each residual pore 15 on the bonding interface 14, and the total length is Σai. The joining rate β (%) can be calculated from α (%) by the equation (2).
α＝Σａｉ／Ｌ×１００＝（ａ１＋ａ２＋・・・＋ａＮ）／Ｌ×１００ ・・・（１）
β＝１００−α ・・・（２）
α = Σai / L × 100 = (a1 + a2 +... + aN) / L × 100 (1)
β = 100−α (2)
そして、内蔵された電極間の耐電圧γは、電極間の離間距離ｃ、接合率β、セラミックス焼結体の耐電圧ｂを用いて、式（３）により簡易的に概算することができる。この算出方法は、セラミックス焼結体１１，１２の材質に関係なく適用することが可能である。 And the withstand voltage γ between the built-in electrodes can be simply estimated by the equation (3) using the separation distance c between the electrodes, the bonding rate β, and the withstand voltage b of the ceramic sintered body. This calculation method can be applied regardless of the material of the ceramic sintered bodies 11 and 12.
γ＝ｂ・ｃ・β／１００ ・・・（３） γ = b · c · β / 100 (3)
発明者は、セラミックス焼結体１１，１２の接合面の表面粗さＲａを０．１μｍ以下とすれば、接合後の接合界面１４に残気孔１５が少ないセラミックス接合体１０が得られることを見い出した。これにより、電極間の耐電圧低下が防止され、高性能な静電チャックを作製することができる。 The inventor has found that if the surface roughness Ra of the bonded surfaces of the ceramic sintered bodies 11 and 12 is 0.1 μm or less, the ceramic bonded body 10 with few residual pores 15 can be obtained at the bonded interface 14 after bonding. It was. Thereby, the withstand voltage drop between electrodes is prevented and a high-performance electrostatic chuck can be manufactured.
接合後の接合界面１４における残気孔１５は、セラミックス焼結体１１，１２の接合面の表面粗さが良好であるほど少なく、セラミックス焼結体１１，１２の接合面の表面粗さＲａは、より好ましくは０．０５μｍ以下である。なお、原料であるセラミックス粉末が９９．９９％の高純度であるとき、不純物が少なくなり、クリープし難くなるが、接合面の表面粗さＲａを０．１μｍ以下とすることにより、電極間の耐電圧低下が防止される程度に、接合後の接合界面１４における残気孔１５が少なくなる。 The residual pores 15 in the bonded interface 14 after bonding are smaller as the surface roughness of the bonded surfaces of the ceramic sintered bodies 11 and 12 is better, and the surface roughness Ra of the bonded surfaces of the ceramic sintered bodies 11 and 12 is More preferably, it is 0.05 μm or less. In addition, when the ceramic powder as the raw material has a high purity of 99.99%, impurities are reduced and creeping is difficult. However, by setting the surface roughness Ra of the bonding surface to 0.1 μm or less, the gap between the electrodes is reduced. The residual pores 15 at the bonded interface 14 after bonding are reduced to such an extent that a decrease in withstand voltage is prevented.
以下、実施例及び比較例を示して、本発明を説明する。 Hereinafter, the present invention will be described with reference to examples and comparative examples.
〔実施例１〜４及び比較例１〜３：酸化アルミニウム焼結体を用いた接合体〕
酸化アルミニウムをセラミックス焼結体として用いた接合体について説明する。
[Examples 1 to 4 and Comparative Examples 1 to 3: Bonded bodies using aluminum oxide sintered bodies]
A bonded body using aluminum oxide as a ceramic sintered body will be described.
［酸化アルミニウム焼結体円板の作製］
原料となる所定純度の酸化アルミニウム粉末に、ＩＰＡ及び有機バインダと可塑剤を添加混合し、スプレードライをすることで酸化アルミニウム顆粒を得た。この顆粒をＣＩＰ成形し、所定の焼成温度で６時間の常圧焼成することで、相対密度９９％以上、φ３００×１０ｍｍの円板形状の酸化アルミニウム焼結体を得た。このようにして得た第１の焼結体及び第２の焼結体に研削、ラッピング加工を施して、板厚１ｍｍ、板厚のばらつきが５μｍ以下、接合面の表面粗さＲｚが平均粒径の１／２以下となるようにした。焼結体の平均粒径は、焼結体の一部を切り出し、切断面のＳＥＭ観察を行って、線インターセプト法により求めた。
[Preparation of aluminum oxide sintered disk]
IPA, an organic binder, and a plasticizer were added to and mixed with aluminum oxide powder having a predetermined purity as a raw material and spray-dried to obtain aluminum oxide granules. The granules were CIP-molded and fired at a predetermined firing temperature for 6 hours under normal pressure to obtain a disk-shaped aluminum oxide sintered body having a relative density of 99% or more and φ300 × 10 mm. The first sintered body and the second sintered body thus obtained were ground and lapped to have a plate thickness of 1 mm, a plate thickness variation of 5 μm or less, and a surface roughness Rz of the joint surface of an average grain. It was made to become 1/2 or less of a diameter. The average particle diameter of the sintered body was determined by a line intercept method by cutting out a part of the sintered body and performing SEM observation of the cut surface.
［導体］
導体としては、Ｍｏ箔を用いた。厚さ０．０５ｍｍ、空隙幅２ｍｍの導体を第１の焼結体に載せた。導体面積は、接合面の７０％とした。
[conductor]
Mo foil was used as the conductor. A conductor having a thickness of 0.05 mm and a gap width of 2 mm was placed on the first sintered body. The conductor area was 70% of the joint surface.
［ホットプレス］
第２の焼結体で導体を挟み込み、ホットプレス冶具にセットした。プレス圧力は１２．５ＭＰa、加熱温度は１４００℃とした。加熱は、第１の焼結体の焼成温度よりも低温で行った。
[hot press]
The conductor was sandwiched between the second sintered bodies and set in a hot press jig. The pressing pressure was 12.5 MPa and the heating temperature was 1400 ° C. The heating was performed at a temperature lower than the firing temperature of the first sintered body.
［評価］
接合部の気密性をボンビング法によりヘリウムリークディテクターで測定し、リーク量が１×１０−７Ｐａ・ｍ３／ｓ以下であれば「○」、それを超えるものは「×」とした。また、接合後の焼結体の粒成長率を切断面のＳＥＭ観察により測定し算出した。
[Evaluation]
The hermeticity of the joint was measured with a helium leak detector by a bombing method. If the leak amount was 1 × 10 −7 Pa · m 3 / s or less, “◯” was given, and if it was more than that, “×” was given. Moreover, the grain growth rate of the sintered compact after joining was measured and calculated by SEM observation of the cut surface.
実施例１〜４では、気密性に優れた接合体が得られた。これらの粒成長率は、いずれも５０％以下であった。また、これらの接合体に内蔵された導体の平面度を渦電流式膜厚計により測定したところ、いずれも５０μｍ以下であった。なお、渦電流式膜厚計による測定では、任意１０箇所について第１の焼結体の厚さを測定し、その最大と最小との差を以って導体の平面度とした。 In Examples 1 to 4, joined bodies having excellent airtightness were obtained. These grain growth rates were all 50% or less. Moreover, when the flatness of the conductor incorporated in these joined bodies was measured with an eddy current film thickness meter, all were 50 μm or less. In the measurement using the eddy current film thickness meter, the thickness of the first sintered body was measured at any 10 locations, and the flatness of the conductor was determined by the difference between the maximum and minimum.
一方、比較例１では、導体の厚さが大きいため気密性が得られなかった。また、比較例２では、第１及び第２の焼結体のいずれの平均粒径も７μｍ以上であったためクリープによる接合に適さず、気密な接合体が得られなかった。比較例３では、導体の厚さに対して空隙幅が小さいため、クリープによる接合ができなかった。 On the other hand, in Comparative Example 1, airtightness was not obtained due to the large conductor thickness. Further, in Comparative Example 2, since the average particle size of each of the first and second sintered bodies was 7 μm or more, it was not suitable for joining by creep, and an airtight joined body could not be obtained. In Comparative Example 3, since the gap width was small with respect to the thickness of the conductor, bonding by creep could not be performed.
［静電チャックの作製］
実施例１について、内部に埋め込まれた導体を基準位置として第１のセラミックス焼結体の厚みを０．３ｍｍまで薄化加工を行った。その後、総厚みが１ｍｍ以下になるように第２のセラミックス焼結体の薄化加工を実施した。その結果、狙いの厚み±１０％の公差で製作できた。
[Production of electrostatic chuck]
About Example 1, the thickness of the 1st ceramic sintered compact was thinned to 0.3 mm by setting the conductor embedded inside as a reference position. Thereafter, the second ceramic sintered body was thinned so that the total thickness was 1 mm or less. As a result, it was possible to manufacture with a target thickness tolerance of ± 10%.
〔実施例５：窒化アルミニウム焼結体を用いた接合体〕
窒化アルミニウムをセラミックス焼結体として用いた接合について説明する。
[Example 5: Joined body using aluminum nitride sintered body]
The joining using aluminum nitride as a ceramic sintered body will be described.
［窒化アルミニウム焼結体円板の作製］
窒化アルミニウム粉末９７質量％、酸化イットリウム粉末３質量％からなる混合粉末にＩＰＡ及び有機バインダと可塑剤を添加混合し、スプレードライをすることで、窒化アルミニウム顆粒を得た。この顆粒をＣＩＰ成形し、所定の焼成温度で６時間の常圧焼成することで、相対密度９９％以上、φ３００×１０ｍｍの円板形状の窒化アルミニウム焼結体を得た。このようにして得た第１及び第２の焼結体に研削、ラッピング加工を施して、板厚２ｍｍ、板厚のばらつきが３μｍ以下、接合面の表面粗さＲｚが平均粒径の１／２以下となるようにした。焼結体の平均粒径は、焼結体の一部を切り出し、切断面のＳＥＭ観察を行って、線インターセプト法により求めた。
[Preparation of aluminum nitride sintered disk]
IPA, an organic binder, and a plasticizer were added to and mixed with a mixed powder composed of 97% by mass of aluminum nitride powder and 3% by mass of yttrium oxide powder, and spray-dried to obtain aluminum nitride granules. The granules were CIP-molded and fired at a predetermined firing temperature for 6 hours under normal pressure to obtain a disc-shaped aluminum nitride sintered body having a relative density of 99% or more and φ300 × 10 mm. The first and second sintered bodies thus obtained are ground and lapped to have a plate thickness of 2 mm, a plate thickness variation of 3 μm or less, and a surface roughness Rz of the joint surface of 1 / average particle diameter. 2 or less. The average particle diameter of the sintered body was determined by a line intercept method by cutting out a part of the sintered body and performing SEM observation of the cut surface.
［導体］
導体としては、Ｍｏメッシュを用いた。線径０．１ｍｍ、＃１００、開口率４７％である。
[conductor]
As a conductor, Mo mesh was used. The wire diameter is 0.1 mm, # 100, and the aperture ratio is 47%.
［ホットプレス］
第２の焼結体で導体を挟み込み、ホットプレス冶具にセットした。プレス圧力は２．５ＭＰａ、加熱温度は１７００℃とした。加熱は、第１及び第２の焼結体の焼成温度よりも低温で行って接合体を得た。
[hot press]
The conductor was sandwiched between the second sintered bodies and set in a hot press jig. The pressing pressure was 2.5 MPa and the heating temperature was 1700 ° C. The heating was performed at a temperature lower than the firing temperature of the first and second sintered bodies to obtain a joined body.
［評価］
接合体に内蔵された導体の平面度を渦電流式膜厚計により測定したところ２５μｍであった。また、接合部の気密度をボンビング法によりヘリウムリークディテクターで測定したところ１×１０−9Ｐａ・ｍ３／ｓであり、気密性は良好であった。また、接合後の焼結体の粒成長率を切断面のＳＥＭ観察により測定し算出したところ、接合前の平均粒径４．２μｍに対し、接合後の平均粒径は、４．８μｍであり、粒成長率は約１４％であった。接合体の総厚さは４ｍｍであり、高精度に導体が内蔵された薄型の窒化珪素セラミックス部材が得られた。なお、渦電流式膜厚計による測定では、任意１０箇所について第１の焼結体の厚さを測定し、その最大と最小との差を以って導体の平面度とした。
[Evaluation]
It was 25 micrometers when the flatness of the conductor incorporated in the joined body was measured with the eddy current film thickness meter. Further, when the air density of the joint was measured by a helium leak detector by a bombing method, it was 1 × 10 −9 Pa · m 3 / s, and the airtightness was good. Further, when the grain growth rate of the sintered body after bonding was measured and calculated by SEM observation of the cut surface, the average particle diameter after bonding was 4.8 μm compared to the average particle diameter before bonding of 4.2 μm. The grain growth rate was about 14%. The total thickness of the joined body was 4 mm, and a thin silicon nitride ceramic member with a built-in conductor with high accuracy was obtained. In the measurement using the eddy current film thickness meter, the thickness of the first sintered body was measured at any 10 locations, and the flatness of the conductor was determined by the difference between the maximum and minimum.
［静電チャックの作製］
得られた接合体について、内部に埋め込まれた導体を基準位置として第１のセラミックス焼結体の厚みを０．１５ｍｍまで薄化加工を行った。その後、総厚みが１ｍｍ以下になるように第２のセラミックス焼結体の薄化加工を実施した。その結果、狙いの厚み±１０％の公差で製作できた。
[Production of electrostatic chuck]
About the obtained joined body, the thickness of the 1st ceramic sintered compact was thinned to 0.15 mm by making the conductor embedded inside the reference position. Thereafter, the second ceramic sintered body was thinned so that the total thickness was 1 mm or less. As a result, it was possible to manufacture with a target thickness tolerance of ± 10%.
〔実施例６：窒化珪素焼結体を用いた接合体〕
窒化珪素をセラミックス焼結体として用いた接合について説明する。
[Example 6: Bonded body using silicon nitride sintered body]
The bonding using silicon nitride as a ceramic sintered body will be described.
［窒化珪素焼結体円板の作製］
窒化珪素粉末９４質量％、酸化イットリウム粉末３質量％、水酸化マグネシウム粉末を酸化マグネシウム換算で３質量％を混合した混合粉末にＩＰＡ及び有機バインダと可塑剤を添加混合し、スプレードライをすることで、窒化珪素顆粒を得た。この顆粒をＣＩＰ成形し、所定の焼成温度で６時間の常圧焼成することで、相対密度９９％以上、φ３００×１０ｍｍの円板形状の窒化珪素焼結体を得た。このようにして得た第１及び第２の焼結体に研削、ラッピング加工を施して、板厚３ｍｍ、板厚のばらつきが１μｍ以下、接合面の表面粗さＲｚが平均粒径の１／２以下となるようにした。焼結体の平均粒径は、焼結体の一部を切り出し、切断面のＳＥＭ観察を行って、線インターセプト法により求めた。
[Preparation of sintered silicon nitride disc]
By adding and mixing IPA, an organic binder and a plasticizer to a mixed powder in which 94% by mass of silicon nitride powder, 3% by mass of yttrium oxide powder, and 3% by mass of magnesium hydroxide powder in terms of magnesium oxide are mixed and spray-dried. A silicon nitride granule was obtained. The granules were CIP-molded and fired at a predetermined firing temperature for 6 hours under normal pressure to obtain a disk-shaped silicon nitride sintered body having a relative density of 99% or more and φ300 × 10 mm. The first and second sintered bodies thus obtained are ground and lapped to have a plate thickness of 3 mm, a plate thickness variation of 1 μm or less, and a surface roughness Rz of the joint surface of 1 / average particle size. 2 or less. The average particle diameter of the sintered body was determined by a line intercept method by cutting out a part of the sintered body and performing SEM observation of the cut surface.
［導体］
導体としては、タングステン薄膜を用いた。厚さ０．０１ｍｍ、空隙幅１ｍｍの導体を第１の焼結体にスパッタリングにより製膜した。導体面積は、接合面の８０％とした。
[conductor]
A tungsten thin film was used as the conductor. A conductor having a thickness of 0.01 mm and a gap width of 1 mm was formed on the first sintered body by sputtering. The conductor area was 80% of the joint surface.
［ホットプレス］
第２の焼結体で導体を挟み込み、ホットプレス冶具にセットした。プレス圧力は０．１ＭＰａ、加熱は１７５０℃とした。
[hot press]
The conductor was sandwiched between the second sintered bodies and set in a hot press jig. The pressing pressure was 0.1 MPa and the heating was 1750 ° C.
［評価］
接合体に内蔵された導体の平面度を渦電流式膜厚計により測定したところ２０μｍであった。また、接合部の気密度をボンビング法によりヘリウムリークディテクターで測定したところ１×１０−9Ｐａ・ｍ３／ｓであり、気密性は良好であった。また、接合後の焼結体の粒成長率を切断面のＳＥＭ観察により測定し算出したところ、接合前の平均粒径５．０μｍに対し、接合後の平均粒径は、７．１μｍであり、粒成長率は４２％であった。接合体の総厚さは６ｍｍであり、高精度に導体が内蔵された薄型の窒化珪素セラミックス部材が得られた。なお、渦電流式膜厚計による測定では、任意１０箇所について第１の焼結体の厚さを測定し、その最大と最小との差を以って導体の平面度とした。
[Evaluation]
It was 20 micrometers when the flatness of the conductor incorporated in the conjugate | zygote was measured with the eddy current type film thickness meter. Further, when the air density of the joint was measured by a helium leak detector by a bombing method, it was 1 × 10 −9 Pa · m 3 / s, and the airtightness was good. Moreover, when the grain growth rate of the sintered body after bonding was measured and calculated by SEM observation of the cut surface, the average particle diameter after bonding was 7.1 μm with respect to the average particle diameter before bonding of 5.0 μm. The grain growth rate was 42%. The total thickness of the joined body was 6 mm, and a thin silicon nitride ceramic member with a built-in conductor with high accuracy was obtained. In the measurement using the eddy current film thickness meter, the thickness of the first sintered body was measured at any 10 locations, and the flatness of the conductor was determined by the difference between the maximum and minimum.
〔静電チャックの作製〕
得られた接合体について、内部に埋め込まれた導体を基準位置として第１のセラミックス焼結体の厚みを０．３ｍｍまで薄化加工を行った。その後、総厚みが１ｍｍ以下になるように第２のセラミックス焼結体の薄化加工を実施した。その結果、狙いの厚み±１０％の公差で製作できた。
[Production of electrostatic chuck]
About the obtained joined body, the thickness of the 1st ceramic sintered compact was thinned to 0.3 mm by using the conductor embedded inside as a reference position. Thereafter, the second ceramic sintered body was thinned so that the total thickness was 1 mm or less. As a result, it was possible to manufacture with a target thickness tolerance of ± 10%.
なお、上記の各実施例では、静電チャックとしたが、これに限るものではなく、導体を発熱抵抗体やＲＦ電極とすることにより、ヒータやサセプタとして適用できる。また、これらを複層に組み合わせて、例えば静電チャック機能付きヒータ等とすることも可能である。 In each of the above-described embodiments, the electrostatic chuck is used. However, the present invention is not limited to this, and the conductor can be applied as a heater or a susceptor by using a heating resistor or an RF electrode. Moreover, it is also possible to combine these in multiple layers to provide, for example, a heater with an electrostatic chuck function.
〔実施例７，８：酸化アルミニウム焼結体を用いた接合体〕
純度９９．９９％の酸化アルミニウムをセラミックス焼結体として用いた接合体について説明する。
[Examples 7 and 8: joined body using aluminum oxide sintered body]
A bonded body using aluminum oxide having a purity of 99.99% as a ceramic sintered body will be described.
［酸化アルミニウム焼結体の作製］
原料となる純度９９．９９％の酸化アルミニウム粉末に、分散剤、バインダ、イオン交換水を添加混合してスラリーを得た。このスラリーを鋳型に注入して真空吸引する鋳込み成形により、成形体を得た。そして、この成形体を所定の焼成温度で２時間の大気常圧焼成することで、相対密度９９％以上、φ３００×５ｍｍの円板形状の酸化アルミニウム焼結体を得た。
[Preparation of sintered aluminum oxide]
A dispersant, a binder, and ion-exchanged water were added to and mixed with aluminum oxide powder having a purity of 99.99% as a raw material to obtain a slurry. A molded body was obtained by casting molding in which this slurry was poured into a mold and vacuum suctioned. Then, this compact was fired at atmospheric pressure for 2 hours at a predetermined firing temperature to obtain a disk-shaped aluminum oxide sintered body having a relative density of 99% or more and φ300 × 5 mm.
こうして得られた焼結体の平均粒径は１〜２μｍであった。なお、平均粒径の値は、焼結体の一部を切り出し、研削、ラッピング加工を施した後、焼成温度の０．９倍程度の温度で、大気常圧で１時間サーマルエッチングを行って得られた試料のラッピング加工面について、ＳＥＭを用いた粒径観測を行い、撮影した写真よりインターセプト法を用いて求めた。 The average particle size of the sintered body thus obtained was 1 to 2 μm. The average particle size is determined by cutting a part of the sintered body, grinding and lapping, and then performing thermal etching for 1 hour at atmospheric pressure at a temperature about 0.9 times the firing temperature. The lapping surface of the obtained sample was subjected to particle size observation using SEM, and determined from the photographed image using the intercept method.
得られた焼結体に研削、ラッピング加工を施して、１辺４０ｍｍ、板厚４ｍｍの正方形板からなり、板厚のばらつきが５μｍ以下の第１及び第２の焼結体を得た。そして、第１及び第２の焼結体の接合面にラッピング加工を行い、実施例７では接合面の表面粗さをＲａ０．０９μｍ、実施例８では接合面の表面粗さをＲａ０．０２μｍと加工した。 The obtained sintered body was ground and lapped to obtain first and second sintered bodies made of a square plate having a side of 40 mm and a plate thickness of 4 mm and having a thickness variation of 5 μm or less. Then, lapping is performed on the bonding surfaces of the first and second sintered bodies. In Example 7, the surface roughness of the bonding surface is Ra 0.09 μm, and in Example 8, the surface roughness of the bonding surface is Ra 0.02 μm. processed.
［導体］
導体として、第２の焼結体のラッピング加工面側に、スクリーン印刷によりＭｏペーストで厚さ９５μｍ、導体間２ｍｍ幅の電極パターンを形成した。Ｍｏペーストは、Ｍｏ粉末にバインダと可塑剤を加え、混合して作製した。
[conductor]
As a conductor, an electrode pattern having a thickness of 95 μm and a width of 2 mm between the conductors was formed by screen printing on the lapping surface side of the second sintered body. The Mo paste was prepared by adding a binder and a plasticizer to the Mo powder and mixing them.
［ホットプレス］
第２の焼結体で導体を挟み込み、ホットプレス冶具にセットした。プレス圧力は９．８ＭＰa、加熱温度は１４００℃とした。
[hot press]
The conductor was sandwiched between the second sintered bodies and set in a hot press jig. The press pressure was 9.8 MPa, and the heating temperature was 1400 ° C.
［評価］
得られたアルミナセラミックス接合体１０について、縦方向に接合体を切断加工し、さらに切断加工面に研削、ラッピング加工を行った。そして、電極間の接合界面を、ＦＥ−ＳＥＭを用いて観察を行った。これによって得られた観察写真により、接合界面１４の残気孔の状況を確認した。
[Evaluation]
About the obtained alumina ceramic joined body 10, the joined body was cut in the vertical direction, and the cut surface was ground and lapped. And the joining interface between electrodes was observed using FE-SEM. The state of residual pores at the bonding interface 14 was confirmed from the observation photograph obtained in this manner.
実施例７で得られたＦＥ−ＳＥＭ観察写真を図３に示す。この写真に基づき、式（１）から、接合界面１４における残気孔率αは３７．３％と求められた。そして、接合率βは式（２）から６２．７％と算出された。 An FE-SEM observation photograph obtained in Example 7 is shown in FIG. Based on this photograph, the residual porosity α at the bonding interface 14 was determined to be 37.3% from the formula (1). And joining rate (beta) was computed with 62.7% from Formula (2).
一般的な酸化アルミニウム焼結体の耐電圧ｂは１３ｋＶ／ｍｍであり、電極間の離間距離ｃを２ｍｍと仮定すると、式（３）から実施例７の電極間の耐電圧γは約１６．３ｋＶと算出された。 Assuming that the withstand voltage b of a general aluminum oxide sintered body is 13 kV / mm and the distance c between the electrodes is 2 mm, the withstand voltage γ between the electrodes of Example 7 is about 16. It was calculated as 3 kV.
酸化アルミニウム焼結体を用いて静電チャックを作製した場合、電極間の耐電圧γが１０ｋＶ以上であれば、十分な絶縁を確保することができることが、発明者のこれまでの知見より分っている。よって、実施例７は電極間の絶縁が十分に確保されており、静電チャックとして良好な性能を発揮できると考えられる。 When an electrostatic chuck is manufactured using an aluminum oxide sintered body, it is understood from the inventors' previous knowledge that sufficient insulation can be secured if the withstand voltage γ between the electrodes is 10 kV or more. ing. Therefore, in Example 7, insulation between the electrodes is sufficiently secured, and it is considered that good performance can be exhibited as an electrostatic chuck.
実施例８で得られたＦＥ−ＳＥＭ観察写真を図４に示す。この写真から明らかなように、接合界面１４に残気孔はほとんど存在せず、残気孔率αは６．８％であった。図３で示した実施例７と比較しても、接合界面１４における残気孔は非常に少なく、残気孔の並びは母材の気孔の並びと比べても遜色がない。 The FE-SEM observation photograph obtained in Example 8 is shown in FIG. As is apparent from this photograph, there were almost no residual pores at the bonding interface 14 and the residual porosity α was 6.8%. Compared with Example 7 shown in FIG. 3, the residual pores at the bonding interface 14 are very few, and the arrangement of the residual pores is not inferior to the arrangement of the pores of the base material.
よって、実施例８は電極間の絶縁が十分に確保されており、静電チャックとして良好な性能を発揮できると考えられる。 Therefore, in Example 8, insulation between the electrodes is sufficiently ensured, and it is considered that good performance as an electrostatic chuck can be exhibited.
１０…接合体、 １１…第１のセラミックス焼結体、 １２…第２のセラミックス焼結体、 １３…導体、 １４…接合界面、 １５…残気孔。 DESCRIPTION OF SYMBOLS 10 ... Bonded body, 11 ... 1st ceramic sintered body, 12 ... 2nd ceramic sintered body, 13 ... Conductor, 14 ... Bonding interface, 15 ... Residual pore.
Claims (8)
前記第１及び第２のセラミックス焼結体の間に前記導体を挟み込み、ホットプレスすることにより、少なくとも一方の前記セラミックス焼結体がクリープして、前記空隙が埋まり、他方の前記セラミックス焼結体と接合する工程と、を含み
前記第１及び第２のセラミックス焼結体は互いに共通する成分を主成分とし、少なくとも一方の前記セラミックス焼結体の平均粒径は７μｍ以下であることを特徴とするセラミックス接合体の製造方法。 A step of preparing first and second ceramic sintered bodies having a relative density of 99% or more, and a conductor having voids;
By sandwiching the conductor between the first and second ceramic sintered bodies and performing hot pressing, at least one of the ceramic sintered bodies creeps to fill the gap, and the other ceramic sintered body The first and second ceramic sintered bodies are composed mainly of components common to each other, and at least one of the ceramic sintered bodies has an average particle size of 7 μm or less. A method for manufacturing a ceramic joined body.
前記第１及び第２のセラミックス焼結体の間には、空隙を有する導体が挟み込まれており、
少なくとも一方の前記セラミックス焼結体がクリープして前記空隙が埋まることにより、他方の前記セラミックス焼結体と接合されたことを特徴とするセラミックス接合体。 A ceramic joined body in which a first ceramic sintered body and a second ceramic sintered body, whose main components are mutually common components, are joined without using a joining material,
A conductor having a gap is sandwiched between the first and second ceramic sintered bodies,
A ceramic joined body which is joined to the other ceramic sintered body by creeping at least one of the ceramic sintered bodies and filling the voids.
The first ceramic sintered body and the second ceramic sintered body having a surface roughness of Ra of 0.1 μm or less are joined to each other, and the first ceramic sintered body and the second ceramic sintered body are joined. An electrostatic chuck comprising the ceramic joined body according to claim 5 or 6, wherein a residual porosity at a joint interface with the bonded body is 40% or less, and the conductor is an electrode.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011148688A (en) * | 2009-12-25 | 2011-08-04 | Taiheiyo Cement Corp | Ceramic joined body and method for producing the same |
| JP2014065631A (en) * | 2012-09-26 | 2014-04-17 | Taiheiyo Cement Corp | Ceramic joined body and method for producing the same |
| WO2015029575A1 (en) * | 2013-08-26 | 2015-03-05 | 京セラ株式会社 | Sample-retainer |
| KR101993110B1 (en) * | 2019-02-28 | 2019-06-25 | 김성환 | Manufacturing Method Of A High-Purity Electrostatic Chuck And Using Press Bonding And the Electrastatic Chuck |
| JPWO2022085307A1 (en) * | 2020-10-21 | 2022-04-28 | ||
| JP7322922B2 (en) | 2020-01-31 | 2023-08-08 | 住友大阪セメント株式会社 | Manufacturing method of ceramic joined body |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04295064A (en) * | 1991-03-22 | 1992-10-20 | Suzuki Motor Corp | Method for joining al2o3-tic combined material |
| JPH0982786A (en) * | 1995-09-19 | 1997-03-28 | Ngk Insulators Ltd | Semiconductor processing apparatus and manufacture thereof |
| JP2002176096A (en) * | 2000-06-30 | 2002-06-21 | Toshiba Ceramics Co Ltd | Manufacturing method of ceramics member for semiconductor treating equipment |
| JP2005022966A (en) * | 2003-06-13 | 2005-01-27 | Tokuyama Corp | Aluminum nitride joined body and its producing method |
| JP2008081362A (en) * | 2006-09-27 | 2008-04-10 | Kwansei Gakuin | Method for producing bonded material of tantalum and carbon, gradient composition structure of tantalum and carbon, method for producing tantalum tube and pit carbon core, tantalum tube and pit carbon core, method for producing tantalum carbide wire, and tantalum carbide wire |
| JP2011148688A (en) * | 2009-12-25 | 2011-08-04 | Taiheiyo Cement Corp | Ceramic joined body and method for producing the same |
-
2010
- 2010-12-24 JP JP2010288674A patent/JP5740637B2/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04295064A (en) * | 1991-03-22 | 1992-10-20 | Suzuki Motor Corp | Method for joining al2o3-tic combined material |
| JPH0982786A (en) * | 1995-09-19 | 1997-03-28 | Ngk Insulators Ltd | Semiconductor processing apparatus and manufacture thereof |
| JP2002176096A (en) * | 2000-06-30 | 2002-06-21 | Toshiba Ceramics Co Ltd | Manufacturing method of ceramics member for semiconductor treating equipment |
| JP2005022966A (en) * | 2003-06-13 | 2005-01-27 | Tokuyama Corp | Aluminum nitride joined body and its producing method |
| JP2008081362A (en) * | 2006-09-27 | 2008-04-10 | Kwansei Gakuin | Method for producing bonded material of tantalum and carbon, gradient composition structure of tantalum and carbon, method for producing tantalum tube and pit carbon core, tantalum tube and pit carbon core, method for producing tantalum carbide wire, and tantalum carbide wire |
| JP2011148688A (en) * | 2009-12-25 | 2011-08-04 | Taiheiyo Cement Corp | Ceramic joined body and method for producing the same |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011148688A (en) * | 2009-12-25 | 2011-08-04 | Taiheiyo Cement Corp | Ceramic joined body and method for producing the same |
| JP2014065631A (en) * | 2012-09-26 | 2014-04-17 | Taiheiyo Cement Corp | Ceramic joined body and method for producing the same |
| WO2015029575A1 (en) * | 2013-08-26 | 2015-03-05 | 京セラ株式会社 | Sample-retainer |
| KR101993110B1 (en) * | 2019-02-28 | 2019-06-25 | 김성환 | Manufacturing Method Of A High-Purity Electrostatic Chuck And Using Press Bonding And the Electrastatic Chuck |
| JP7322922B2 (en) | 2020-01-31 | 2023-08-08 | 住友大阪セメント株式会社 | Manufacturing method of ceramic joined body |
| JPWO2022085307A1 (en) * | 2020-10-21 | 2022-04-28 | ||
| JP7388573B2 (en) | 2020-10-21 | 2023-11-29 | 住友大阪セメント株式会社 | Ceramic bonded body, electrostatic chuck device, manufacturing method of ceramic bonded body |
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