JP4912544B2 - Low thermal conductivity high rigidity ceramics - Google Patents
Low thermal conductivity high rigidity ceramics Download PDFInfo
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- JP4912544B2 JP4912544B2 JP2001210292A JP2001210292A JP4912544B2 JP 4912544 B2 JP4912544 B2 JP 4912544B2 JP 2001210292 A JP2001210292 A JP 2001210292A JP 2001210292 A JP2001210292 A JP 2001210292A JP 4912544 B2 JP4912544 B2 JP 4912544B2
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Description
【０００１】
【発明の属する技術分野】
本発明は、低熱伝導性で、かつ高剛性なセラミックスに関わるものである。
【０００２】
【従来の技術】
近年、高い剛性、寸法安定性、化学的安定性などの特長を利用して、半導体製造装置用、精密機器用、計測機器用などの部品として、各種のセラミックスが使用されるようになってきた。例えば、半導体製造工程の露光装置におけるサセプタ、真空チャック、ＸＹテーブル、ミラー等にはアルミナ、窒化珪素、炭化珪素などのセラミックスが用いられるようになってきている。
【０００３】
これらは、高い剛性、寸法安定性、化学的安定性などの特長を利用しているものであるが、一方、半導体検査装置の中には検査部と他の部分との断熱性を確保するために低熱伝導性の素材であって、かつ、高精度を確保するためにたわまず高剛性を有する素材が要求されている。
【０００４】
【発明が解決しようとする課題】
アルミナの場合、剛性は高いが、熱伝導率はセラミックスの中でも比較的大きい方であり、こういった断熱性を要求する用途には向かないのが現状である。一方、ジルコニアは優れた断熱性を有するが、焼成の際に約３０％も収縮するため、焼成変形を起こしやすいという課題がある。さらに、ジルコニアは難削材であり、精密な形状付与に仕上げる焼結体加工には時間がかかり、コストも高くなるという問題もあった。次に、断熱性に富み、加工性の高いマシナブルセラミックスやガラス材料は剛性が低く、たわみが生じるため、この用途には向かないという課題があった。
本発明は、以上の点に鑑み成されたものであり、従来の技術では不可能であった、低熱伝導性を有するとともに、高いヤング率を示すセラミックスを提供することを目的としたものである。
【０００５】
上記した本発明の目的は、ユークリプタイト６０〜８０体積％とＴｉＯ2２０〜４０体積％とからなり、理論密度の９５％以上の緻密体であり、室温における熱伝導率が３Ｗ／ｍ・Ｋ未満であり、かつヤング率が１４０ＧＰａ以上であることを特徴とする低熱伝導高剛性セラミックスによって達成される。
【０００６】
また、当該目的は、ユークリプタイト４０〜７０体積％とＺｒＯ2３０〜６０体積％とからなり、理論密度の９５％以上の緻密体であり、室温における熱伝導率が３Ｗ／ｍ・Ｋ未満であり、かつヤング率が１４０ＧＰａ以上であることを特徴とする低熱伝導高剛性セラミックスによっても達成される。
【０００７】
【発明の実施の形態】
本発明による低熱伝導高剛性セラミックスは、ユークリプタイトとＴｉＯ2またはＺｒＯ2との複合セラミックスである。ここで、ユークリプタイトをＴｉＯ2との複合化の場合には６０〜８０体積％、ＺｒＯ2との複合化の場合には４０〜７０体積％含有させる理由は、ユークリプタイトが複合セラミックスの熱伝導を低下させるための重要な成分であるが、ユークリプタイトの量が前記限定した体積％を越えて多いと今度はヤング率が低くなるため好ましくなくなり、逆に、ユークリプタイトの量が前記限定した体積％を越えて少ないと熱伝導性が高くなり好ましくないからである。
【０００８】
また、本発明の複合セラミックスはＴｉＯ2であれば２０〜４０体積％、また、ＺｒＯ2であれば３０〜６０体積％の割合で含有するものである。
ここで、前記含有割合未満ではヤング率が低くなるため好ましくなく、前記含有割合を超えると、熱伝導率が大きくなるため好ましくない。また、ＴｉＯ2の結晶系はルチル型、アナターゼ型いずれでも良い。また、ＺｒＯ2はＹ2Ｏ3、ＣａＯ、ＭｇＯ等で安定化したものが望ましい。
【０００９】
本発明のセラミックスは、熱伝導率が低い一方で、ヤング率の低いユークリプタイトと熱伝導率が比較的低いものの、ヤング率の高いＴｉＯ2またはＺｒＯ2を複合化して得られるものである。従って、セラミックスの断熱性を重視するには、ユークリプタイトの含有量を多くし、ヤング率のほうを重視するのであれば、ＴｉＯ2またはＺｒＯ2の含有量を増やせば良い。
【００１０】
本発明の複合セラミックスを作製するには、ユークリプタイト粉末と、ＴｉＯ2またはＺｒＯ2を原料粉末として用意する。用いるユークリプタイト、及び、ＴｉＯ2、ＺｒＯ2粉末は平均粒径０.1〜５μm程度であるのが均一混合されやすく、焼結しやすいので好ましい。また、これら原料中には緻密化を進めるために助剤の役割を果たす不純物、例えばアルカリ並びにアルカリ土類金属酸化物、あるいはそれらの化合物などが含有されていても構わないが、その含有量は焼結して得られた複合セラミックスの５重量％以下、特に２重量％以下が好ましい。なぜなら、これより多いとガラス相が形成されて、ヤング率が低下するため好ましくないからである。
【００１１】
各原料を配合し、エタノール、水、トルエン等の溶媒を加え、別々にボールミルなどにより十分に混合し、乾燥して、出発原料粉を得る。得られた出発原料粉を所定形状に所望の成形手段、例えば、金型プレス、ラバープレス、冷間静水圧プレス等により任意の形状に成形後、焼成する。なお、これら乾式成形法の他に、押し出し成形法、鋳込み成形法、射出成形法などを適宜選択することが出来る。
【００１２】
焼成は、空気中で１１００〜１５５０℃、好ましくは１２００〜１４００℃の温度範囲で１〜１０時間程度焼結することにより緻密化することができる。
ここで、焼成温度が１１００℃よりも低いと緻密化が困難であり、１５５０℃を越えると成形体が溶融するため好ましくない。
【００１３】
以上説明した本発明によれば、理論密度が９５％以上と緻密体であり、室温における室温における熱伝導率が３Ｗ／ｍ・Ｋ未満であり、かつヤング率が１４０ＧＰａ以上という優れた特性を有する複合セラミックスが得られる。
【００１４】
以下、本発明の実施例と比較例とを具体的に挙げ、本発明をより詳細に説明するが、本発明はこれらにより何ら制限されるのものではない。
【００１５】
（１）複合セラミックスの作製
平均粒径４μｍの市販のユークリプタイト粉末と表１に示したＴｉＯ2またはＺｒＯ2粉末または比較例としてのＡｌ2Ｏ3粉末とを、種々の配合割合となるよう精秤して配合原料とした。この配合原料粉末１００重量部にエタノールを１００重量部加えて、２４時間混合粉砕した後、エバポレーターで乾燥した。得られた混合粉末を金型プレスにて５０×５０×１０ｍｍの大きさになるよう、１０ＭＰａで予備成形した上、冷間静水圧プレスにて１００ＭＰａの圧力で成形した。次に、成形体を空気中、１３５０℃で３時間焼成して、複合セラミックスを得た。
【００１６】
【表１】
（２）評価
得られた複合セラミックスから試験片を切り出し、密度、熱伝導率、ヤング率を測定した。密度はアルキメデス法、熱伝導率はレーザーフラッシュ法（ＪＩＳＲ１６１１「ファインセラミックスのレーザーフラッシュ法による熱拡散率・比熱容量・熱伝導率試験方法」）、ヤング率は共振法（ＪＩＳ Ｒ１６０２「ファインセラミックスの弾性率試験方法」）を用いて測定した。それらの結果を表２にまとめて示した。（ここで、表中の配合量とは配合物の配合量を体積％で示したものであって、残部はユークリプタイトである。）
【００１８】
【表２】
表２の結果より、本発明による複合セラミックス（実施例１〜５）はいずれも理論密度が９５％以上であり、室温における室温における熱伝導率が３Ｗ／ｍ・Ｋ未満であり、かつヤング率が１４０ＧＰａ以上であった。これは、比較例１〜３では得ることができない優れた特性を有するものである。
すなわち、熱伝導率はジルコニアの３.１Ｗ/ｍ・Ｋより低く断熱性が高く、ヤング率はマシナブルセラミックスより高剛性であった。したがって、本発明の複合セラミックスであれば、既存のセラミックス材料より加重に対して変形の小さい断熱部材としての適用が可能であることが分かった。
【００２０】
【発明の効果】
本発明のセラミックスは、上記したように低熱伝導性を維持しつつ、剛性の高いものである。従って、これにより検査部を断熱しながら効率的に測定を行うことができ、優れた検査精度が得られる。したがって、半導体素子製造の品質と量産性を格段に高めることができた。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to ceramics having low thermal conductivity and high rigidity.
[0002]
[Prior art]
In recent years, various ceramics have come to be used as parts for semiconductor manufacturing equipment, precision equipment, measuring equipment, etc. by utilizing features such as high rigidity, dimensional stability, and chemical stability. . For example, ceramics such as alumina, silicon nitride, and silicon carbide have been used for susceptors, vacuum chucks, XY tables, mirrors, and the like in exposure apparatuses in semiconductor manufacturing processes.
[0003]
These utilize features such as high rigidity, dimensional stability, and chemical stability. On the other hand, in semiconductor inspection equipment, in order to ensure heat insulation between the inspection part and other parts. In addition, a material having a low rigidity and a high rigidity is required to ensure high accuracy.
[0004]
[Problems to be solved by the invention]
In the case of alumina, the rigidity is high, but the thermal conductivity is relatively large among ceramics, so that it is not suitable for applications requiring such heat insulation. On the other hand, zirconia has excellent heat insulating properties, but shrinks as much as about 30% during firing, so that there is a problem that firing deformation is likely to occur. Furthermore, zirconia is a difficult-to-cut material, and there has been a problem that it takes time and costs to process the sintered body to give a precise shape. Next, machinable ceramics and glass materials, which are highly heat-insulating and have high workability, have a problem that they are not suitable for this application because of their low rigidity and deflection.
The present invention has been made in view of the above points, and an object thereof is to provide a ceramic having low thermal conductivity and high Young's modulus, which is impossible with conventional techniques. .
[0005]
An object of the present invention described above, eucryptite 60-80 vol% and Ri Do from the TiO 2 20 to 40 vol%, 95% or more dense body of theoretical density, thermal conductivity at room temperature is 3W / m It is achieved by a low thermal conductivity high rigidity ceramic characterized by being less than K and having a Young's modulus of 140 GPa or more .
[0006]
Furthermore, the object is Yuktobanian descriptor Ri Do from the tight 40-70 vol% and ZrO 2 30 to 60 vol%, 95% or more dense body of theoretical density, thermal conductivity at room temperature is 3W / m · K It is also achieved by a low-heat-conductivity and high-rigidity ceramic characterized by having a Young's modulus of 140 GPa or more .
[0007]
DETAILED DESCRIPTION OF THE INVENTION
The low thermal conductivity high rigidity ceramic according to the present invention is a composite ceramic of eucryptite and TiO 2 or ZrO 2 . Here, 60 to 80% by volume of eucryptite in the case of composite with TiO 2 and 40 to 70% by volume in the case of composite with ZrO 2 are the reason why eucryptite is contained in the composite ceramic. Although it is an important component for lowering heat conduction, if the amount of eucryptite exceeds the limited volume%, the Young's modulus will be lowered this time. This is because if the amount exceeds the limited volume%, the thermal conductivity becomes high, which is not preferable.
[0008]
The composite ceramic of the present invention contains 20 to 40% by volume of TiO 2 and 30 to 60% by volume of ZrO 2 .
Here, if the content is less than the above-described content, the Young's modulus is low, which is not preferable. The crystal system of TiO 2 may be either a rutile type or an anatase type. ZrO 2 is preferably stabilized with Y 2 O 3 , CaO, MgO or the like.
[0009]
The ceramic of the present invention is obtained by combining eucryptite having a low Young's modulus with a low Young's modulus and TiO 2 or ZrO 2 having a high Young's modulus while having a relatively low thermal conductivity. Therefore, in order to emphasize the heat insulating property of ceramics, if the content of eucryptite is increased and the Young's modulus is more important, the content of TiO 2 or ZrO 2 may be increased.
[0010]
In order to produce the composite ceramic of the present invention, eucryptite powder and TiO 2 or ZrO 2 are prepared as raw material powders. The eucryptite and TiO 2 and ZrO 2 powders to be used preferably have an average particle size of about 0.1 to 5 μm because they are easily mixed and easily sintered. In addition, these raw materials may contain impurities that act as auxiliary agents to promote densification, such as alkali and alkaline earth metal oxides, or compounds thereof, but the content is The composite ceramic obtained by sintering is preferably 5% by weight or less, particularly preferably 2% by weight or less. This is because if it is more than this, a glass phase is formed and the Young's modulus is lowered, which is not preferable.
[0011]
Each raw material is blended, a solvent such as ethanol, water, toluene, etc. is added, separately mixed well by a ball mill or the like, and dried to obtain a starting raw material powder. The obtained starting raw material powder is formed into a desired shape by a desired forming means such as a die press, a rubber press, a cold isostatic press and the like, and then fired. In addition to these dry molding methods, extrusion molding methods, cast molding methods, injection molding methods, and the like can be selected as appropriate.
[0012]
Firing can be densified by sintering in air at a temperature of 1100 to 1550 ° C, preferably 1200 to 1400 ° C for about 1 to 10 hours.
Here, if the firing temperature is lower than 1100 ° C., densification is difficult, and if it exceeds 1550 ° C., the molded body is melted, which is not preferable.
[0013]
According to the present invention described above, the theoretical density is 95% or more, a dense body, the thermal conductivity at room temperature at room temperature is less than 3 W / m · K, and the Young's modulus is 140 GPa or more. A composite ceramic is obtained.
[0014]
Hereinafter, although the Example and comparative example of this invention are mentioned concretely and this invention is demonstrated in detail, this invention is not restrict | limited at all by these.
[0015]
(1) Production of composite ceramics Commercial eucryptite powder having an average particle diameter of 4 μm and TiO 2 or ZrO 2 powder shown in Table 1 or Al 2 O 3 powder as a comparative example are mixed in various proportions. It was precisely weighed and used as a blended raw material. 100 parts by weight of ethanol was added to 100 parts by weight of the blended raw material powder, mixed and ground for 24 hours, and then dried with an evaporator. The obtained mixed powder was preformed at 10 MPa so as to have a size of 50 × 50 × 10 mm by a mold press and then molded at a pressure of 100 MPa by a cold isostatic press. Next, the compact was fired in air at 1350 ° C. for 3 hours to obtain a composite ceramic.
[0016]
[Table 1]
(2) Evaluation A test piece was cut out from the obtained composite ceramic, and the density, thermal conductivity, and Young's modulus were measured. Density is Archimedes method, thermal conductivity is laser flash method (JISR1611 “Test method of thermal diffusivity, specific heat capacity, thermal conductivity of fine ceramics by laser flash method”), Young's modulus is resonance method (JIS R1602 “elasticity of fine ceramics”) Rate test method "). The results are summarized in Table 2. (Here, the blending amount in the table indicates the blending amount of the blend in volume%, and the balance is eucryptite.)
[0018]
[Table 2]
From the results of Table 2, the composite ceramics according to the present invention (Examples 1 to 5) all have a theoretical density of 95% or more, a thermal conductivity at room temperature at room temperature of less than 3 W / m · K, and a Young's modulus. Was 140 GPa or more. This has excellent characteristics that cannot be obtained in Comparative Examples 1 to 3.
That is, the thermal conductivity was lower than 3.1 W / m · K of zirconia and the heat insulation was high, and the Young's modulus was higher than that of machinable ceramics. Therefore, it was found that the composite ceramic of the present invention can be applied as a heat insulating member having a smaller deformation with respect to load than existing ceramic materials.
[0020]
【Effect of the invention】
As described above, the ceramic of the present invention has high rigidity while maintaining low thermal conductivity. Accordingly, it is possible to efficiently perform the measurement while insulating the inspection portion, and excellent inspection accuracy can be obtained. Therefore, the quality and mass productivity of semiconductor device manufacturing can be greatly improved.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2001210292A JP4912544B2 (en) | 2001-07-11 | 2001-07-11 | Low thermal conductivity high rigidity ceramics |
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| JP2001210292A JP4912544B2 (en) | 2001-07-11 | 2001-07-11 | Low thermal conductivity high rigidity ceramics |
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| JP4912544B2 true JP4912544B2 (en) | 2012-04-11 |
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| US7696116B2 (en) | 2006-03-23 | 2010-04-13 | Colorado School Of Mines | Implementing a pressure-induced phase transformation in beta-eucryptite to impart toughening |
| ES2362533B1 (en) * | 2009-12-21 | 2012-05-17 | Consejo Superior De Investigaciones Cientificas (Csic) | COMPOSITE MATERIAL WITH THERMAL EXPANSION COEFFICIENT CONTROLLED WITH OXIDIC MICAS CERAMICS AND THEIR OBTAINING PROCEDURE. |
| FR2959506B1 (en) * | 2010-04-30 | 2014-01-03 | Thales Sa | CERAMIC COMPOSITE MATERIAL BASED ON BETA-EUCRYPTITE AND OXIDE AND PROCESS FOR THE PRODUCTION OF SAID MATERIAL |
| WO2018008379A1 (en) * | 2016-07-06 | 2018-01-11 | 日本電気硝子株式会社 | Composite ceramic powder, sealing material, and composite ceramic powder production method |
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| JPH0829977B2 (en) * | 1990-04-05 | 1996-03-27 | 岐阜県 | High strength / low thermal expansion ceramic and method for manufacturing the same |
| JP4261631B2 (en) * | 1998-03-11 | 2009-04-30 | 京セラ株式会社 | Manufacturing method of ceramic sintered body |
| JP4658312B2 (en) * | 2000-12-06 | 2011-03-23 | 京セラ株式会社 | Lithium aluminosilicate ceramics |
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