JP3676552B2 - Low thermal expansion ceramics and method for producing the same - Google Patents
Low thermal expansion ceramics and method for producing the same Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、真空装置構造体、サセプタ、静電チャックあるいはステージや半導体製造プロセスにおける治具などに適したコージェライトを主体とする低熱膨張セラミックスとその製造方法に関する。
【０００２】
【従来技術】
従来より、コージェライト系焼結体は、従来から低熱膨張のセラミックスとして知られており、フィルター、ハニカム、耐火物などに応用されている。このコージェライト系焼結体は、コージェライト粉末、あるいはコージェライトを形成するＭｇＯ、Ａｌ2 Ｏ3 、ＳｉＯ2 粉末を配合して、これに焼結助剤として、希土類元素酸化物や、ＳｉＯ2 、ＣａＯ、ＭｇＯなどを添加し、所定形状に成形後、１０００〜１４００℃の温度で焼成することによって作製される（特公昭５７−３６２９号、特開平２−２２９７６０号）。
【０００３】
一方、ＬＳＩなどの半導体装置の製造工程において、シリコンウエハに配線を形成する工程において、ウエハを支持または保持するためのサセプタ、静電チャックや絶縁リングとしてあるいはその他の治具等として、これまでアルミナや窒化珪素が比較的に安価で、化学的にも安定であるため広く用いられている。また、露光装置のＸＹテーブル等として従来よりアルミナや窒化珪素などのセラミックスも用いられている。
【０００４】
また、最近では、コージェライトの低熱膨張性を利用し、半導体製造装置用部品として応用することが、特開平１−１９１４２２号や特公平６−９７６７５号にて提案されている。特開平１−１９１４２２号によれば、Ｘ線マスクにおけるマスク基板に接着する補強リングとして、ＳｉＯ2 、インバーなどに加え、コージェライトによって形成しメンブレンの応力を制御することが提案されている。
【０００５】
また、特公平６−９７６７５号では、ウエハを載置する静電チャック用基盤としてアルミナやコージェライト系焼結体を使用することが提案されている。
【０００６】
【発明が解決しようとする課題】
近年、ＬＳＩなどにおける高集積化に伴い、回路の微細化が急速に進められ、その線幅もサブミクロンオーダーのレベルまで高精密化しつつある。そしてＳｉウエハに高精密回路を形成するための露光装置に対して高い精度が要求され、たとえば露光装置のステージ用部材においては１００ｎｍ（０．１μｍ）以下の位置決め精度が要求され、露光の位置合わせ誤差が製品の品質向上や歩留まり向上に大きな影響を及ぼしているのが現状である。
【０００７】
半導体製造装置用として一般に用いられてきたアルミナ、窒化珪素などのセラミックスは、金属に比べて熱膨張率が小さいものの、１０〜４０℃の熱膨張率はそれぞれ５．２×１０-6／℃、１．５×１０-6／℃であり、雰囲気温度が０．１℃変化すると数１００ｎｍ（０．１μｍ）の変形が発生することになり、露光等の精密な工程ではこの変化が大きな問題となり、従来のセラミックスでは精度が低く、生産性の低下をもたらしている。
【０００８】
これに対して、コージェライト系焼結体は、熱膨張率が０．２×１０-6／℃程度と、アルミナや窒化珪素に比較して熱膨張率が低く、上記のような露光精度に対する問題はある程度解決される。
【０００９】
ところが、露光装置のステージのように、Ｓｉウエハを載置した支持体が露光処理を施す位置まで高速移動を伴うような場合には、移動後の支持体自体が所定位置に停止後も振動しており、そのために、その振動した状態で露光処理を施すと露光精度が低下するという問題があった。これは、露光によって形成する配線幅が細くなるほど顕著であり、高微細な配線回路を形成する上では致命的な問題となっていた。
【００１０】
このような振動は、部材自体の剛性が低いことによって引き起こされるものであることから、これらの部材に対しては高い剛性、即ち高ヤング率が要求されている。
【００１１】
従って、本発明は、それ自体低熱膨張を有するとともに、高剛性を有する低熱膨張セラミックスとその製造方法を提供することを目的とするものである。また、本発明は、ステージなどの高速駆動される場合においても振動が生じにくい半導体製造用部品を提供することを目的とするものである。
【００１２】
【課題を解決するための手段】
本発明者等は、上記課題に対し鋭意研究を重ねた結果、コージェライトに希土類元素酸化物を所定の比率で複合化し、かつコージェライト結晶の粒界に前記希土類元素酸化物を特定の結晶相として存在させることにより、低熱膨張特性を阻害することなく焼結性を高め、ヤング率を高めることができることを見いだし、本発明に至った。
【００１３】
即ち、本発明の低熱膨張セラミックスは、コージェライトを８０〜９２重量％、Ｙ、Ｙｂ、Ｅｒ及びＣｅからなる群より選択された希土類元素（ＲＥ）の酸化物を８〜２０重量％の割合で含み、相対密度９５％以上であり、且つコージェライト結晶の粒界に、ＲＥ２Ｏ３・２ＳｉＯ２で表されるダイシリケート結晶相が析出しており、１３０ＧＰａ以上のヤング率を有していることを特徴とするものであり、さらに、低熱膨張セラミックスの製造方法としては、コージェライト粉末を８０〜９２重量％、Ｙ、Ｙｂ、Ｅｒ及びＣｅからなる群より選択された希土類元素（ＲＥ）の酸化物を８〜２０重量％の割合で配合した成形体を、１３００〜１５００℃の温度で焼成した後、１０００℃までを１０℃／ｍｉｎ以下の冷却速度で冷却し、ＲＥ ２ Ｏ ３ ・２ＳｉＯ ２ で表されるダイシリケート結晶相を析出せしめることを特徴とするものである。
【００１４】
【発明の実施の形態】
本発明の低熱膨張セラミックスは、コージェライトは、一般式２ＭｇＯ・２Ａｌ2 Ｏ3 ・５ＳｉＯ2 で表される複合酸化物を主体とするものであり、平均粒径が１〜１０μｍの結晶粒子として存在する。このコージェライトは、焼結体中に、８０〜９２重量％、好ましくは８５〜９０重量％の割合で存在する。
【００１５】
また、この焼結体中には、副成分として希土類元素酸化物を８〜２０重量％、特に１０〜１５重量％の割合で含有するものである。希土類元素酸化物は、焼成時にコージェライトの成分と反応し、液相を生成することから焼結性を高める作用が発揮されるとともにそれ自体のヤング率が高いために、これらを含有せしめることにより、後述する実施例から明らかなように、焼結体のヤング率を１３０ＧＰａ以上に高めることができる。
【００１６】
このような希土類元素酸化物の添加により、焼結体の相対密度を９５％以上、特に９６％以上まで高めることができる。焼結助剤量が８重量％よりも少ないと焼結性が十分でなく、高い温度で焼成する必要があり、または相対密度９５％以上に緻密化できなくなる。また２０重量％を越えると熱膨張係数が大きくなり、０．５×１０-6／℃以下の特性が達成できない。
【００１７】
また、焼結体中には、上記のコージェライト結晶粒子の粒界に、焼結助剤として添加された希土類元素（ＲＥ）酸化物がＲＥ２Ｏ３・２ＳｉＯ２で表されるダイシリケート結晶相として存在することによって、セラミックスの熱膨張率が大きくなることを防ぐことができる。即ち、希土類元素酸化物が、粒界において、非晶質相として存在する場合に比較して、結晶相、とりわけＲＥ２Ｏ３・２ＳｉＯ２で表されるダイシリケート相は、原子配列が密であるために、焼結体全体のヤング率を向上させるとともに、熱膨張係数も低下させる作用を有する。なお、希土類元素としては、Ｙ、Ｙｂ、ＥｒあるいはＣｅが使用される。
【００１８】
上記のように、粒界にダイシリケート結晶相を析出させるためには、希土類元素酸化物を比較的多量に含有することが必要である。従って、希土類元素酸化物の含有量を上記の比率に限定したのは、８重量％よりも少ないとダイシリケート結晶相の析出が望めず、その結果、セラミックスのヤング率を高めることができず、２０重量％よりも大きいと反応するコージェライトの量が多くなるとともに異相が析出し、セラミックスの熱膨張率が大きくなり、コージェライトの優れた低熱膨張特性が発揮されないためである。なお、本発明のセラミックスの熱膨張率は、１０〜４０℃において０．５×１０-6／℃以下、特に０．４×１０-6／℃以下であるのが望ましい。
【００１９】
かかるダイシリケート結晶相は、希土類元素酸化物と、コージェライト中のＳｉＯ2 分との反応により生成される結晶相であるが、コージェライト結晶相は、必ずしも一般式２ＭｇＯ・２Ａｌ2 Ｏ3 ・５ＳｉＯ2 の組成からなるものではなく、ＭｇＯ、Ａｌ2 Ｏ3 、ＳｉＯ2 の各成分に対して固溶源が大きいために、例えば、希土類元素酸化物と反応した残余のＭｇＯ、Ａｌ2 Ｏ3 は、コージェライト結晶中に固溶して、非化学量論組成のコージェライト結晶相を形成してもよい。
【００２０】
上記のようなセラミックスを作製するには、平均粒径が１０μｍ以下のコージェライト粉末に対して、平均粒径が１０μｍ以下の希土類元素酸化物粉末を８〜２０重量％の割合で添加する。
【００２１】
上記の比率で各成分を配合した後、ボールミルなどにより十分に混合し、所定形状に所望の成形手段、例えば、金型プレス，冷間静水圧プレス，押出し成形等により任意の形状に成形後、焼成する。
【００２２】
焼成は、１３００〜１５００℃の温度範囲、好ましくは１３５０〜１４５０℃で１〜１０時間程度焼結することにより相対密度９８％以上に緻密化することができる。このときの温度が１３００℃よりも低いと緻密化できず、１５００℃を越えると、成形体が溶融してしまう。
【００２３】
また、本発明において、粒界にＲＥ2 Ｏ3 ・２ＳｉＯ2 の結晶相を析出させるためには、上記の焼成後に焼成温度から１０００℃の温度領域までを平均で１０℃／ｍｉｎ以下、特に５℃／ｍｉｎ以下の冷却速度で冷却することが必要である。この温度領域の冷却速度が１０℃／ｍｉｎよりも速いと粒界にダイシリケート結晶相を析出させることは困難である。なお、徐冷温度領域は、焼成温度から１０００℃以下の領域まで拡げても何ら差し支えない。
【００２４】
【実施例】
平均粒径が３μｍのコージェライト粉末に対して、平均粒径が１μｍのＹ2 Ｏ3 、Ｙｂ2 Ｏ3 、Ｅｒ2 Ｏ3 、ＣｅＯ2 の各粉末を表１、表２に示す割合で調合後、ボールミルで２４時間混合した後、１ｔ／ｃｍ2 の圧力で金型成形した。そして、その成形体を炭化珪素質の匣鉢に入れて表１、２の条件で焼成し、１０００℃までの平均冷却速度を表１、２のように変化させて実施して、種々のセラミックスを作製した。
【００２５】
得られたセラミックスを研磨し、３×４×１５ｍｍの大きさに研削加工し、このセラミックスの１０〜４０℃までの熱膨張係数を測定した。また、超音波パルス法により、室温でのヤング率を測定した。結果は表１，２に示した。
【００２６】
【表１】
【表２】
表１，２にみられるように、本発明に基づき、コージェライトに希土類元素酸化物を所定比率で添加し、ＲＥ2 Ｏ3 ・２ＳｉＯ2 の結晶相を析出させることにより、熱膨張率の低減化を図り０．５×１０-6／℃以下を達成し、且つヤング率を１２０ＧＰａ以上に高めることができ、その添加量が増加するに従いヤング率が高くなる傾向が見られた。
【００２９】
しかし、これらの希土類元素酸化物量が８重量％よりも少ない試料Ｎo.１は、相対密度９５％以上が達成されず、しかもヤング率が１２０ＧＰａよりも低く、熱膨張率も０．５×１０-6／℃よりも大きいものであった。また、２０重量％を越える試料Ｎo.１７では、ヤング率は高いものの熱膨張率が０．５×１０-6／℃よりも大きいものであった。
【００３０】
さらに、焼成温度については、１３００℃よりも低い試料Ｎo.３では緻密化することができず相対密度９５％以上が達成されなかった。また、焼成温度が１５００℃よりも高い試料Ｎo.９では、成形体の溶融が見られ、セラミックスを作製することができなかった。
【００３１】
また、冷却速度については、１０００℃までの冷却速度が１０℃／ｍｉｎよりも速い試料Ｎo.１３、１４、２２、２７、３２では、ＲＥ2 Ｏ3 ・２ＳｉＯ2 の結晶相が析出せず、その結果、ヤング率が低く、しかも熱膨張係数も大きいものであった。従って、粒界にＲＥ2 Ｏ3 ・２ＳｉＯ2 の結晶相を析出させることが高ヤング率化、低熱膨張化の上で重要であることがわかる。
【００３２】
【発明の効果】
以上詳述した通り、本発明の低熱膨張セラミックスは、コージェライトの優れた低熱膨張特性を維持しつつ、剛性、即ち、ヤング率を高めることができる。その結果、この低熱膨張セラミックスを高微細な回路を形成するためのウエハに露光処理を行うなどの半導体製造装置用部品、例えば、露光装置用ステージなどとして用いることにより、雰囲気の温度変化に対しても寸法の変化がなく、優れた精度が得られるとともに、振動に伴う精度の低下をも防止することができ、半導体素子製造の品質と量産性を高めることができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a low thermal expansion ceramic mainly composed of cordierite suitable for a vacuum device structure, a susceptor, an electrostatic chuck, a stage, a jig in a semiconductor manufacturing process, and the like, and a manufacturing method thereof.
[0002]
[Prior art]
Conventionally, cordierite-based sintered bodies are conventionally known as low thermal expansion ceramics and are applied to filters, honeycombs, refractories, and the like. This cordierite-based sintered body is blended with cordierite powder or MgO, Al 2 O 3 , and SiO 2 powder forming cordierite, and a rare earth element oxide or SiO 2 as a sintering aid. , CaO, MgO, etc. are added, formed into a predetermined shape, and then fired at a temperature of 1000 to 1400 ° C. (Japanese Examined Patent Publication No. 57-3629, Japanese Laid-Open Patent Application No. 2-229760).
[0003]
On the other hand, in the manufacturing process of semiconductor devices such as LSI, in the process of forming wiring on a silicon wafer, as a susceptor, electrostatic chuck, insulating ring or other jig for supporting or holding the wafer, alumina has been used so far. And silicon nitride are widely used because they are relatively inexpensive and chemically stable. In addition, ceramics such as alumina and silicon nitride are conventionally used as an XY table for an exposure apparatus.
[0004]
Recently, it has been proposed in Japanese Patent Application Laid-Open No. 1-191422 and Japanese Patent Publication No. 6-97675 to utilize the low thermal expansion property of cordierite as a component for a semiconductor manufacturing apparatus. According to Japanese Patent Laid-Open No. 1-191422, it is proposed that a reinforcing ring bonded to a mask substrate in an X-ray mask is formed by cordierite in addition to SiO 2 or invar to control the membrane stress.
[0005]
Japanese Patent Publication No. 6-97675 proposes the use of alumina or a cordierite-based sintered body as an electrostatic chuck substrate on which a wafer is placed.
[0006]
[Problems to be solved by the invention]
In recent years, along with higher integration in LSIs and the like, circuit miniaturization has been rapidly progressed, and the line width is also being improved to a submicron order level. Further, high accuracy is required for an exposure apparatus for forming a high-precision circuit on a Si wafer. For example, a stage member of the exposure apparatus requires positioning accuracy of 100 nm (0.1 μm) or less, and exposure alignment is performed. The current situation is that errors greatly affect the quality improvement and yield improvement of products.
[0007]
Although ceramics such as alumina and silicon nitride that have been generally used for semiconductor manufacturing equipment have a smaller coefficient of thermal expansion than metals, the coefficient of thermal expansion at 10 to 40 ° C. is 5.2 × 10 −6 / ° C., respectively. It is 1.5 × 10 -6 / ° C. When the ambient temperature changes by 0.1 ° C, deformation of several hundreds of nanometers (0.1 µm) occurs, and this change becomes a major problem in precise processes such as exposure. Conventional ceramics have low accuracy, resulting in a decrease in productivity.
[0008]
On the other hand, the cordierite-based sintered body has a thermal expansion coefficient of about 0.2 × 10 −6 / ° C., which is lower than that of alumina or silicon nitride. The problem is solved to some extent.
[0009]
However, when the support on which the Si wafer is placed is moved to a position where exposure processing is performed, such as the stage of an exposure apparatus, the support itself after the movement vibrates even after stopping at a predetermined position. For this reason, there has been a problem in that the exposure accuracy is lowered when the exposure process is performed in the vibrated state. This is more conspicuous as the width of the wiring formed by exposure becomes narrower, and has become a fatal problem in forming a highly fine wiring circuit.
[0010]
Since such vibration is caused by the low rigidity of the members themselves, high rigidity, that is, high Young's modulus is required for these members.
[0011]
Accordingly, an object of the present invention is to provide a low thermal expansion ceramic that has low thermal expansion and high rigidity, and a method for producing the same. Another object of the present invention is to provide a semiconductor manufacturing component that is less prone to vibration even when driven at a high speed, such as a stage.
[0012]
[Means for Solving the Problems]
As a result of intensive studies on the above problems, the present inventors have complexed rare earth element oxides with cordierite at a predetermined ratio, and the rare earth element oxides have a specific crystal phase at the grain boundaries of the cordierite crystals. As a result, the present inventors have found that it is possible to enhance the sinterability and increase the Young's modulus without hindering the low thermal expansion characteristics, and have reached the present invention.
[0013]
That is, the low thermal expansion ceramic of the present invention comprises cordierite in an amount of 80 to 92% by weight, rare earth element (RE) oxide selected from the group consisting of Y, Yb, Er and Ce in a proportion of 8 to 20% by weight. And a relative density of 95% or more, and a disilicate crystal phase represented by RE 2 O 3 · 2SiO 2 is precipitated at the grain boundary of the cordierite crystal and has a Young's modulus of 130 GPa or more. it is characterized in further process for producing a low thermal expansion ceramics, cordierite powder 80 to 92 wt%, Y, Yb, rare earth element selected from the group consisting of Er and Ce of (RE) the molded body obtained by blending the oxide in a proportion of 8-20 wt.%, after firing at a temperature of 1300 to 1500 ° C., until 1000 ° C. and cooled in the following cooling rate 10 ° C. / min, R It is characterized in that the allowed to precipitate disilicate crystal phase represented by 2 O 3 · 2SiO 2.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
In the low thermal expansion ceramic of the present invention, cordierite is mainly composed of a composite oxide represented by the general formula 2MgO · 2Al 2 O 3 · 5SiO 2 and exists as crystal particles having an average particle size of 1 to 10 μm. To do. This cordierite is present in the sintered body in a proportion of 80 to 92% by weight, preferably 85 to 90% by weight.
[0015]
The sintered body contains rare earth element oxide as an auxiliary component in an amount of 8 to 20% by weight, particularly 10 to 15% by weight. Rare earth element oxides react with the cordierite components during firing to produce a liquid phase, so that the effect of enhancing the sinterability is exhibited and the Young's modulus of itself is high. As is apparent from the examples described later, the Young's modulus of the sintered body can be increased to 130 GPa or more .
[0016]
By adding such a rare earth element oxide, the relative density of the sintered body can be increased to 95% or more, particularly 96% or more. If the amount of the sintering aid is less than 8% by weight, the sinterability is not sufficient, it is necessary to fire at a high temperature, or the relative density cannot be increased to 95% or more. On the other hand, if it exceeds 20% by weight, the coefficient of thermal expansion becomes large, and characteristics of 0.5 × 10 −6 / ° C. or less cannot be achieved.
[0017]
Further, in the sintered body, a disilicate crystal in which a rare earth element (RE) oxide added as a sintering aid is represented by RE 2 O 3 · 2SiO 2 at the grain boundary of the cordierite crystal particles. By existing as a phase, it is possible to prevent an increase in the coefficient of thermal expansion of the ceramic. That is, compared to the case where the rare earth element oxide exists as an amorphous phase at the grain boundary, the crystal phase, particularly the disilicate phase represented by RE 2 O 3 · 2SiO 2 has a dense atomic arrangement. Therefore, it has the effect of improving the Young's modulus of the entire sintered body and reducing the thermal expansion coefficient. Note that Y, Yb, Er, or Ce is used as the rare earth element.
[0018]
As described above, in order to precipitate the disilicate crystal phase at the grain boundary, it is necessary to contain a relatively large amount of rare earth element oxide. Therefore, the content of the rare earth element oxide is limited to the above-mentioned ratio. If the content is less than 8% by weight, precipitation of a disilicate crystal phase cannot be expected, and as a result, the Young's modulus of the ceramic cannot be increased. When the amount is more than 20% by weight, the amount of cordierite that reacts increases and a heterogeneous phase precipitates, the thermal expansion coefficient of the ceramic increases, and the excellent low thermal expansion characteristic of cordierite is not exhibited. The thermal expansion coefficient of the ceramic of the present invention is desirably 0.5 × 10 −6 / ° C. or less, particularly 0.4 × 10 −6 / ° C. or less at 10 to 40 ° C.
[0019]
Such a disilicate crystal phase is a crystal phase formed by a reaction between a rare earth element oxide and a SiO 2 component in cordierite, but the cordierite crystal phase is not necessarily a general formula 2MgO · 2Al 2 O 3 · 5SiO. 2 and a large solid solution source for each component of MgO, Al 2 O 3 and SiO 2 , for example, the residual MgO and Al 2 O 3 reacted with the rare earth element oxide are The cordierite crystal phase having a non-stoichiometric composition may be formed by solid solution in the cordierite crystal.
[0020]
In order to produce the ceramic as described above, a rare earth element oxide powder having an average particle size of 10 μm or less is added at a ratio of 8 to 20% by weight to a cordierite powder having an average particle size of 10 μm or less.
[0021]
After blending each component in the above ratio, mix well with a ball mill or the like, and after molding into a desired shape by a desired molding means such as a die press, cold isostatic pressing, extrusion molding, etc., Bake.
[0022]
Firing can be densified to a relative density of 98% or more by sintering at a temperature range of 1300 to 1500 ° C., preferably 1350 to 1450 ° C. for about 1 to 10 hours. If the temperature at this time is lower than 1300 ° C., it cannot be densified, and if it exceeds 1500 ° C., the molded body will melt.
[0023]
In the present invention, in order to precipitate the RE 2 O 3 .2SiO 2 crystal phase at the grain boundaries, the average from the firing temperature to the temperature range of 1000 ° C. after the firing is 10 ° C./min or less, particularly 5 It is necessary to cool at a cooling rate of ° C./min or less. If the cooling rate in this temperature region is faster than 10 ° C./min, it is difficult to precipitate a disilicate crystal phase at the grain boundary. The slow cooling temperature region can be expanded from the firing temperature to a region of 1000 ° C. or lower.
[0024]
【Example】
Each powder of Y 2 O 3 , Yb 2 O 3 , Er 2 O 3 , and CeO 2 having an average particle size of 1 μm is prepared in the proportions shown in Tables 1 and 2 with respect to the cordierite powder having an average particle size of 3 μm. Then, after mixing for 24 hours with a ball mill, the mold was molded at a pressure of 1 t / cm 2 . Then, the molded body was put in a silicon carbide mortar and fired under the conditions shown in Tables 1 and 2, and the average cooling rate up to 1000 ° C. was changed as shown in Tables 1 and 2 to implement various ceramics. Was made.
[0025]
The obtained ceramic was polished and ground to a size of 3 × 4 × 15 mm, and the thermal expansion coefficient of this ceramic up to 10 to 40 ° C. was measured. Further, the Young's modulus at room temperature was measured by an ultrasonic pulse method. The results are shown in Tables 1 and 2.
[0026]
[Table 1]
[Table 2]
As can be seen from Tables 1 and 2 , the thermal expansion coefficient is reduced by adding rare earth element oxides to cordierite at a predetermined ratio and precipitating a crystal phase of RE 2 O 3 .2SiO 2 based on the present invention. achieving the aims 0.5 × 10 -6 / ℃ or less of, and can increase the Young's modulus over 120 GPa, a tendency that the Young's modulus increases were observed in accordance with the addition amount increases.
[0029]
However, sample No. 1 in which the amount of these rare earth element oxides is less than 8% by weight does not achieve a relative density of 95% or more, has a Young's modulus lower than 120 GPa, and a thermal expansion coefficient of 0.5 × 10 −. It was larger than 6 / ° C. In Sample No. 17 exceeding 20% by weight, the Young's modulus was high, but the thermal expansion coefficient was larger than 0.5 × 10 −6 / ° C.
[0030]
Furthermore, regarding the firing temperature, the sample No. 3 lower than 1300 ° C. could not be densified, and a relative density of 95% or more was not achieved. Further, in sample No. 9 having a firing temperature higher than 1500 ° C., the molded body was melted, and ceramics could not be produced.
[0031]
As for the cooling rate, in the samples No. 13, 14, 22, 27, and 32 where the cooling rate up to 1000 ° C. is faster than 10 ° C./min, the crystal phase of RE 2 O 3 .2SiO 2 does not precipitate, As a result, the Young's modulus was low and the coefficient of thermal expansion was large. Therefore, it can be seen that the precipitation of the RE 2 O 3 .2SiO 2 crystal phase at the grain boundaries is important for increasing the Young's modulus and reducing the thermal expansion.
[0032]
【The invention's effect】
As described above in detail, the low thermal expansion ceramic of the present invention can increase rigidity, that is, Young's modulus, while maintaining the excellent low thermal expansion characteristics of cordierite. As a result, by using this low thermal expansion ceramic as a component for semiconductor manufacturing equipment such as performing exposure processing on a wafer for forming a high-definition circuit, for example, a stage for an exposure equipment, the temperature of the atmosphere can be reduced. In addition, there is no change in dimensions, and excellent accuracy can be obtained. Also, a decrease in accuracy due to vibration can be prevented, and the quality and mass productivity of semiconductor element manufacturing can be improved.
Claims (2)
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29276597A JP3676552B2 (en) | 1997-10-24 | 1997-10-24 | Low thermal expansion ceramics and method for producing the same |
| US09/177,977 US6265334B1 (en) | 1997-10-24 | 1998-10-22 | Ceramic sintered product and process for producing the same |
| DE19849340A DE19849340B4 (en) | 1997-10-24 | 1998-10-26 | Ceramic sintered product and process for its production |
| DE19861434A DE19861434B4 (en) | 1997-10-24 | 1998-10-26 | An article of low thermal expansion ceramic material and its use |
| US10/124,067 USRE39120E1 (en) | 1997-10-24 | 2002-04-16 | Ceramic sintered product and process for producing the same |
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| Application Number | Priority Date | Filing Date | Title |
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| JP29276597A JP3676552B2 (en) | 1997-10-24 | 1997-10-24 | Low thermal expansion ceramics and method for producing the same |
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| Publication Number | Publication Date |
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| JPH11130520A JPH11130520A (en) | 1999-05-18 |
| JP3676552B2 true JP3676552B2 (en) | 2005-07-27 |
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| JP29276597A Expired - Fee Related JP3676552B2 (en) | 1997-10-24 | 1997-10-24 | Low thermal expansion ceramics and method for producing the same |
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| JP2002167267A (en) * | 2000-11-28 | 2002-06-11 | Kyocera Corp | Low thermal expansion ceramic and method of manufacturing it |
| US7960009B2 (en) * | 2008-02-29 | 2011-06-14 | Corning Incorporated | Dispersion-toughened cordierite for filter and substrate applications |
| JP5657210B2 (en) | 2009-01-28 | 2015-01-21 | 京セラ株式会社 | A member for semiconductor manufacturing equipment comprising a cordierite sintered body |
| JP2010208943A (en) * | 2010-05-17 | 2010-09-24 | Kyocera Corp | Low thermal expansion ceramic and method for producing the same |
| EP2679562B1 (en) | 2011-02-24 | 2017-03-29 | Kyocera Corporation | Cordierite sintered body and member for semiconductor device composed of cordierite sintered body |
| JP6231910B2 (en) * | 2014-03-14 | 2017-11-15 | 日本碍子株式会社 | Plugged honeycomb structure |
| JP6940959B2 (en) * | 2016-03-23 | 2021-09-29 | 日本碍子株式会社 | Cordellite sintered body, its manufacturing method and composite substrate |
| CN115974540B (en) * | 2022-12-03 | 2023-11-24 | 昆明理工大学 | Rare earth doped cordierite ceramic material and preparation method thereof |
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