JP2003048771A - Low thermal expansion ceramics and method of manufacturing the same - Google Patents
Low thermal expansion ceramics and method of manufacturing the sameInfo
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- JP2003048771A JP2003048771A JP2001234669A JP2001234669A JP2003048771A JP 2003048771 A JP2003048771 A JP 2003048771A JP 2001234669 A JP2001234669 A JP 2001234669A JP 2001234669 A JP2001234669 A JP 2001234669A JP 2003048771 A JP2003048771 A JP 2003048771A
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、低熱膨張セラミッ
クスおよびその製造方法に関するもので、さらに詳しく
は、低熱膨張でかつ高剛性であり半導体製造工程等に好
適に用いられる低熱膨張セラミックスおよびその製造方
法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to low thermal expansion ceramics and a method for producing the same, and more specifically, low thermal expansion ceramics having low thermal expansion and high rigidity, which are suitable for use in semiconductor manufacturing processes and the like, and a method for producing the same. It is about.
【０００２】[0002]
【従来の技術】近年、半導体製造装置、精密機器、計測
機器等の部品として、セラミックスが広く使用されてき
ている。例えば、半導体ウエハを指示するサセプタ、真
空チャック、絶縁リング等には、従来アルミナ、窒化珪
素、炭化珪素などのセラミックスが用いられていた。最
近ではＬＳＩなどの高度集積化の要求により、製造現場
での温度変化の影響を受けにくいユークリプタイトやコ
ージエライトなどの熱膨張の小さいセラミックスが用い
られるようになってきている。2. Description of the Related Art In recent years, ceramics have been widely used as parts for semiconductor manufacturing equipment, precision instruments, measuring instruments and the like. For example, ceramics such as alumina, silicon nitride, and silicon carbide have been conventionally used for a susceptor, a vacuum chuck, an insulating ring, and the like for indicating a semiconductor wafer. Recently, due to the demand for high integration of LSIs and the like, ceramics such as eucryptite and cordierite, which are not easily affected by temperature changes at the manufacturing site, have come to be used.
【０００３】しかし、これらのセラミックスは、熱膨張
係数は小さいものの、剛性は十分でなく外的な応力によ
り歪むため、例えば露光装置のテーブル部材として使用
する場合、振動等によるのテーブルの変形により精密な
位置決めができないという問題点があった。したがっ
て、本出願人は、熱膨張係数が負の値を有するユークリ
プタイト５０〜９５体積％と熱膨張係数が正であり高剛
性を有するα−ＳｉＣ、β−ＳｉＣ、Ｓｉ3Ｎ4、ＴｉＢ
2、ＺｒＢ2、ＷＣ、ＴｉＣ、ＺｒＮから選ばれる１種以
上の化合物５〜５０体積％とを複合させることによって
低熱膨張でかつ高剛性なセラミックスが得られることに
着目して既に出願を行っている。However, although these ceramics have a small coefficient of thermal expansion, they do not have sufficient rigidity and are distorted by external stress. Therefore, when they are used as a table member of an exposure apparatus, they are precisely deformed by the table due to vibration or the like. There was a problem that it could not be positioned correctly. Therefore, the applicant of the present invention has found that eucryptite having a negative thermal expansion coefficient of 50 to 95% by volume and positive thermal expansion coefficient of α-SiC, β-SiC, Si 3 N 4 , and TiB having high rigidity.
The application has already been filed, paying attention to the fact that by combining 5 to 50% by volume of one or more compounds selected from 2 , ZrB 2 , WC, TiC, and ZrN, ceramics with low thermal expansion and high rigidity can be obtained. There is.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、本出願
人が提案した低熱膨張セラミックスは、相対密度を９８
％以上に高密度化することが難しく、高密度化するため
には相対密度９０％以上となるように常圧焼結した後
に、１００気圧以上で高圧焼結する必要があった。これ
は、本出願人が提案した低熱膨張セラミックスの緻密化
温度と溶融温度が近接しているため、常圧焼結のみによ
り相対密度を９８％以上に高密度化しようとすると緻密
化が完了する前に一部が溶融してしまうという課題があ
ったためである。したがって、焼結工程と緻密化工程の
２工程が必要となり、量産効率が悪いという問題点があ
った。However, the low thermal expansion ceramics proposed by the present applicant has a relative density of 98.
%, It was difficult to densify it to a high density, and in order to densify it, it was necessary to sinter under normal pressure so that the relative density would be 90% or higher, and then under high pressure at 100 atm or higher. This is because the densification temperature and the melting temperature of the low thermal expansion ceramics proposed by the present applicant are close to each other, so that the densification is completed when the relative density is increased to 98% or more only by the atmospheric pressure sintering. This is because there was a problem that some of them melted before. Therefore, two steps, a sintering step and a densification step, are required, which causes a problem of poor mass production efficiency.
【０００５】[0005]
【課題を解決するための手段】本出願人は前記した問題
点を解決するために鋭意検討した結果、セラミックス中
に含まれるＦｅ2Ｏ3の含有量が０．０５重量％以下とな
るように各製造工程を制御することにより常圧焼結のみ
でも相対密度９８％以上と高密度化できることに着目し
て本発明を完成したものである。すなわち、本発明の目
的は、常圧焼結のみでも相対密度９８％以上と高密度化
できる低熱膨張セラミックスおよびその製造方法に係わ
る技術を提供することを目的としている。Means for Solving the Problems As a result of intensive studies for solving the above-mentioned problems, the present applicant has found that the content of Fe 2 O 3 contained in ceramics should be 0.05% by weight or less. The present invention has been completed by focusing on the fact that the relative density can be increased to 98% or more only by pressureless sintering by controlling each manufacturing process. That is, an object of the present invention is to provide a technique related to a low thermal expansion ceramics which can be densified to a relative density of 98% or more even by pressureless sintering alone, and a technique relating to a manufacturing method thereof.
【０００６】上記した本発明の目的は、ユークリプタイ
ト５０〜９５体積％、並びにα−ＳｉＣ、β−ＳｉＣ、
Ｓｉ3Ｎ4、ＴｉＢ2、ＺｒＢ2、ＷＣ、ＴｉＣ、ＺｒＮか
ら選ばれる１種以上の化合物５〜５０体積％を含有する
低熱膨張セラミックスであって、前記セラミックス中に
含まれるＦｅ2Ｏ3の含有量が０．０５重量％以下である
ことを特徴とする低熱膨セラミックスによって達成され
る。また、セラミックスの相対密度が９８％以上、室温
でのヤング率が１２０ＧＰａ以上、１０〜４０℃におけ
る熱膨張係数が−１〜１×１０-6／℃以下であることを
特徴とする前記の低熱膨セラミックスによって達成され
る。さらに本発明の目的は、セラミックス中のＦｅ2Ｏ3
の含有量が０．０５重量％以下となるように各製造工程
を制御しながら、ユークリプタイト５０〜９５体積％、
並びにα−ＳｉＣ、β−ＳｉＣ、Ｓｉ3Ｎ4、ＴｉＢ2、
ＺｒＢ2、ＷＣ、ＴｉＣ、ＺｒＮから選ばれる１種以上
の化合物５〜５０体積％からなる成形体を真空または不
活性ガス雰囲気中で１１００〜１５５０℃の温度で焼結
させることを特徴とする低熱膨張セラミックスの製造方
法によって達成される。The above-mentioned objects of the present invention are 50 to 95% by volume of eucryptite, α-SiC, β-SiC,
Si 3 N 4, TiB 2, ZrB 2, WC, TiC, a low thermal expansion ceramics containing 5-50 vol% of one or more compounds selected from ZrN, of Fe 2 O 3 contained in the ceramics This is achieved by the low thermal expansion ceramics characterized in that the content is 0.05% by weight or less. In addition, the relative density of ceramics is 98% or more, the Young's modulus at room temperature is 120 GPa or more, and the coefficient of thermal expansion at 10 to 40 ° C. is −1 to 1 × 10 −6 / ° C. or less. Achieved by expanded ceramics. A further object of the present invention is to provide Fe 2 O 3 in ceramics.
While controlling each manufacturing process so that the content of eucryptite is 0.05% by weight or less, 50 to 95% by volume of eucryptite,
And α-SiC, β-SiC, Si 3 N 4 , TiB 2 ,
Low heat, characterized by sintering a molded body composed of 5 to 50% by volume of one or more compounds selected from ZrB 2 , WC, TiC and ZrN at a temperature of 1100 to 1550 ° C. in a vacuum or an inert gas atmosphere. This is achieved by the method for producing expanded ceramics.
【０００７】[0007]
【発明の実施の形態】本発明のセラミックスでは、ユー
クリプタイト５０〜９５体積％、並びにα−ＳｉＣ、β
−ＳｉＣ、Ｓｉ3Ｎ4、ＴｉＢ2、ＺｒＢ2、ＷＣ、Ｔｉ
Ｃ、ＺｒＮから選ばれる１種以上の化合物５〜５０体積
％を含有する低熱膨張である。その理由は、ユークリプ
タイトが５０体積％未満では熱膨張率が高くなり、９５
体積％を越えるとヤング率が低くなり（剛性が小さくな
り）好ましくないからである。BEST MODE FOR CARRYING OUT THE INVENTION In the ceramics of the present invention, 50-95% by volume of eucryptite, α-SiC, β
-SiC, Si 3 N 4, TiB 2, ZrB 2, WC, Ti
Low thermal expansion containing 5 to 50% by volume of one or more compounds selected from C and ZrN. The reason is that when eucryptite is less than 50% by volume, the coefficient of thermal expansion becomes high, and
This is because the Young's modulus becomes low (rigidity becomes low) when it exceeds the volume%, which is not preferable.
【０００８】また本発明では、セラミックスの相対密度
が９８％以上、室温でのヤング率が１２０ＧＰａ以上、
１０〜４０℃における熱膨張係数が−１〜１×１０-6／
℃以下であることを特徴とする低熱膨セラミックスを提
案している。その理由は、密度が緻密化していないと強
度が低下したり、耐食性が劣るからであり、ヤング率が
低いと剛性が小さいため歪みやすくなるからであり、ま
た、熱膨張係数が低くないと製造現場の温度変化を受け
て高集積化した半導体装置の製造には好ましくなくなる
からである。Further, in the present invention, the relative density of the ceramics is 98% or more, the Young's modulus at room temperature is 120 GPa or more,
Thermal expansion coefficient at 10 to 40 ° C is -1 to 1 x 10 -6 /
We have proposed a low thermal expansion ceramics, which is characterized by being below ℃. The reason is that if the density is not densified, the strength is reduced, or the corrosion resistance is inferior, and if the Young's modulus is low, the rigidity is low and the strain is likely to occur. This is because it becomes unfavorable for manufacturing highly integrated semiconductor devices due to temperature changes in the field.
【０００９】また、本発明ではセラミックス中のＦｅ2
Ｏ3の含有量が０．０５重量％以下となるように各製造
工程を制御している。これは、Ｆｅ2Ｏ3が本発明のセラ
ミックスの融点を他の不純物にも増して低下させ緻密化
温度と溶融温度を近接させる作用があり、したがって、
緻密化を効率的に行うためにはＦｅ2Ｏ3の含有量を制御
することが重要となるからである。ここで、セラミック
ス中のＦｅ2Ｏ3の含有量を０．０５重量％以下とした理
由は、これにより融点温度をＦｅ2Ｏ3の含有量制御前の
１３５０℃から１３９０℃まで高めることができ、１３
７０℃の常圧焼結のみでも相対密度９８％以上の緻密な
セラミックスを得ることができるからである。Further, in the present invention, Fe 2 in the ceramic is
Each manufacturing process is controlled so that the content of O 3 is 0.05% by weight or less. This is because Fe 2 O 3 has a function of lowering the melting point of the ceramics of the present invention more than other impurities to bring the densification temperature and the melting temperature close to each other, and therefore,
This is because it is important to control the content of Fe 2 O 3 for efficient densification. Here, the reason why the content of Fe 2 O 3 in the ceramics is 0.05% by weight or less is that the melting point temperature can be increased from 1350 ° C. before controlling the content of Fe 2 O 3 to 1390 ° C. , 13
This is because a dense ceramic having a relative density of 98% or more can be obtained only by normal pressure sintering at 70 ° C.
【００１０】次に、セラミックス中のＦｅ2Ｏ3の含有量
が０．０５重量％以下となるように制御するに際して
は、原料粉末調整工程、成形工程、焼成工程、加工工程
の各製造工程において、Ｆｅ2Ｏ3の含有量が限定した値
を越えないように抑制することが重要であり、このう
ち、原料粉末調整工程の制御には他の工程より特別の注
意を払う必要がある。すなわち、高純度の原料粉末を準
備するのと同時に原料粉末の混練時にＦｅ2Ｏ3の混入を
避けるように特別な配慮をすることが好ましい。Next, when controlling the content of Fe 2 O 3 in the ceramics to be not more than 0.05% by weight, the raw material powder adjusting step, the molding step, the firing step, and the processing step should be performed. , Fe 2 O 3 It is important to suppress the content of Fe 2 O 3 so as not to exceed the limited value. Among these, the control of the raw material powder adjusting step requires special attention than the other steps. That is, it is preferable to take special consideration so as to avoid mixing Fe 2 O 3 when kneading the raw material powders at the same time as preparing the high-purity raw material powders.
【００１１】さらに、本出願人が提案したセラミックス
中のＦｅ2Ｏ3の含有量を０．０５重量％以下とすると、
セラミックスの比透磁率を１．０００以下とすることが
可能となり、磁性を帯びた材料を使用できない電子線描
画装置用の材料としては好適に使用できるようになると
いう効果もある。なぜなら、電子線描画装置のマスクホ
ルダー等に使用する場合、比透磁率が１．０００を越え
て大きい材料を使用すると、電子線が磁性により影響を
受けて描画精度を低下させて好ましくないという課題が
あったからである。Further, when the content of Fe 2 O 3 in the ceramics proposed by the applicant is set to 0.05% by weight or less,
It is also possible to make the relative magnetic permeability of the ceramics 1.000 or less, and it is possible to suitably use the material as a material for an electron beam drawing apparatus in which a magnetic material cannot be used. This is because when used in a mask holder or the like of an electron beam drawing apparatus, if a material having a relative magnetic permeability exceeding 1.000 is used, the electron beam is affected by magnetism and the drawing accuracy is lowered, which is not preferable. Because there was.
【００１２】以下に、本発明を実施例と比較例により詳
細に説明するが、本発明は実施例に限定されるものでは
ない。
（１）複合セラミックスの製造方法
平均粒径４μｍ以下の市販の高純度のユークリプタイト
粉末、および、表１に示したα−ＳｉＣ、β−ＳｉＣ、
Ｓｉ3Ｎ4、ＴｉＢ2、ＺｒＢ2、ＷＣ、ＴｉＣ、ＺｒＮ粉
末を出発原料として種々の割合に配合し、配合原料を作
成した。この配合原料粉末１００重量部に有機系結合剤
２重量部を加えて、2４時間混合粉砕した。得られた粉
末を５０×５０×１０ｍｍの大きさに１０ＭＰａで予備
成形した後、１００ＭＰａで冷間静水圧プレスで成形を
行った。この成形体を、窒素雰囲気において５００℃で
脱脂した後、アルゴン雰囲気中で１３７０℃で焼成し、
複合セラミックスを得た。比較例として高純度でない市
販のユークリプタイト粉末を用いて実施例と同様の条件
で得られた成形体についてもアルゴン雰囲気中で１３４
０℃と１３７０℃で焼結を行った。The present invention will be described in detail below with reference to examples and comparative examples, but the present invention is not limited to the examples. (1) Method for producing composite ceramics Commercially available high-purity eucryptite powder having an average particle size of 4 μm or less, and α-SiC and β-SiC shown in Table 1.
Si 3 N 4, TiB 2, ZrB 2, WC, TiC, and formulated into various proportions ZrN powder as a starting material to prepare a mixed material. To 100 parts by weight of this blended raw material powder, 2 parts by weight of an organic binder was added and mixed and pulverized for 24 hours. The obtained powder was preformed into a size of 50 × 50 × 10 mm at 10 MPa, and then subjected to cold isostatic pressing at 100 MPa. This molded body was degreased at 500 ° C. in a nitrogen atmosphere and then fired at 1370 ° C. in an argon atmosphere,
A composite ceramic was obtained. As a comparative example, a molded body obtained by using a commercially available eucryptite powder having a high purity and under the same conditions as in the example was used in an argon atmosphere.
Sintering was performed at 0 ° C and 1370 ° C.
【００１３】[0013]
【表１】 [Table 1]
【００１４】（２）評価
次に、得られた焼結体から試験片を切り出し、相対密度
はアルキメデス法により、熱膨張係数はレーザ熱膨張計
により、ヤング率はＪＩＳＲ１６０２に規定された方法
により、比透磁率は磁気天秤法により、体積抵抗率はＪ
ＩＳ Ｃ２１４１に規定された方法により測定した。ま
た、各焼結体に含まれるＦｅ2Ｏ3の含有量についても公
知の分析方法により測定した。得られた評価結果を表２
にまとめて示した。（ここで、Ｎｏ．１〜１０は本発明
の実施例で比１と比２は比較例である。）(2) Evaluation Next, a test piece was cut out from the obtained sintered body, the relative density was measured by the Archimedes method, the thermal expansion coefficient was measured by a laser thermal expansion meter, and the Young's modulus was measured by the method specified in JISR1602. The relative permeability is measured by the magnetic balance method, and the volume resistivity is J
It was measured by the method specified in IS C2141. The content of Fe 2 O 3 contained in each sintered body was also measured by a known analysis method. Table 2 shows the obtained evaluation results.
Are summarized in. (Here, Nos. 1 to 10 are examples of the present invention, and ratios 1 and 2 are comparative examples.)
【００１５】[0015]
【表２】 [Table 2]
【００１６】表２の結果から明らかなように、本発明に
よるものは相対密度が９８％以上と高密度であり、しか
も、室温でのヤング率が１２０ＧＰａ以上、１０〜４０
℃における熱膨張係数が−１〜１×１０-6／℃以下とな
った。さらには、比透磁率を１．０００以下とすること
が可能となり、磁性を帯びた材料を使用できない電子線
描画装置用の材料として好適に使用できることを確認し
た。一方、比較例２では溶融し、緻密な焼結体を得るこ
とができなかった。また、焼成温度を下げて焼結した比
較例１では、密度が低く、しかも比透磁率は１．０００
を越えた値となった。As is clear from the results shown in Table 2, according to the present invention, the relative density is as high as 98% or more, and the Young's modulus at room temperature is 120 GPa or more, 10-40.
The coefficient of thermal expansion at ℃ became -1 to 1 × 10 -6 / ℃ or less. Furthermore, it has been confirmed that the relative magnetic permeability can be set to 1.000 or less, and that the material can be suitably used as a material for an electron beam drawing apparatus in which a magnetic material cannot be used. On the other hand, in Comparative Example 2, it was melted and a dense sintered body could not be obtained. In Comparative Example 1 in which the firing temperature was lowered, the density was low and the relative magnetic permeability was 1.000.
The value exceeded.
【００１７】[0017]
【発明の効果】以上説明したように、本発明によれば、
高剛性を有する低熱膨張セラミックスを常圧焼結のみで
も相対密度９８％以上に高密度化できるという効果があ
る。As described above, according to the present invention,
There is an effect that the relative density of the low thermal expansion ceramics having high rigidity can be increased to 98% or more only by the normal pressure sintering.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 菊地 真哉 千葉県佐倉市大作２−４−２ 太平洋セメ ント株式会社中央研究所内 Ｆターム(参考） 4G030 AA02 AA45 AA47 AA49 AA52 AA54 BA24 GA24 GA27 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Shinya Kikuchi 2-4-2 Daisaku Sakura City, Chiba Prefecture Pacific Semé Central Research Institute F-term (reference) 4G030 AA02 AA45 AA47 AA49 AA52 AA54 BA24 GA24 GA27
Claims (3)
びにα−ＳｉＣ、β−ＳｉＣ、Ｓｉ3Ｎ4、ＴｉＢ2、Ｚ
ｒＢ2、ＷＣ、ＴｉＣ、ＺｒＮから選ばれる１種以上の
化合物５〜５０体積％を含有する低熱膨張セラミックス
であって、前記セラミックス中に含まれるＦｅ2Ｏ3の含
有量が０．０５重量％以下であることを特徴とする低熱
膨セラミックス。1. Eucryptite 50 to 95% by volume, and α-SiC, β-SiC, Si 3 N 4 , TiB 2 , Z.
rB 2, WC, TiC, a low thermal expansion ceramics containing 5-50 vol% of one or more compounds selected from ZrN, the content of Fe 2 O 3 contained in said ceramic 0.05 wt% A low thermal expansion ceramics characterized by being:
室温でのヤング率が１２０ＧＰａ以上、１０〜４０℃に
おける熱膨張係数が−１〜１×１０-6／℃以下であるこ
とを特徴とする請求項１記載の低熱膨セラミックス。2. The relative density of ceramics is 98% or more,
The low thermal expansion ceramics according to claim 1, wherein the Young's modulus at room temperature is 120 GPa or more and the thermal expansion coefficient at 10 to 40 ° C is -1 to 1 x 10 -6 / ° C or less.
０．０５重量％以下となるように各製造工程を制御しな
がら、ユークリプタイト５０〜９５体積％、並びにα−
ＳｉＣ、β−ＳｉＣ、Ｓｉ3Ｎ4、ＴｉＢ2、ＺｒＢ2、Ｗ
Ｃ、ＴｉＣ、ＺｒＮから選ばれる１種以上の化合物５〜
５０体積％からなる成形体を真空または不活性ガス雰囲
気中で１１００〜１５５０℃の温度で焼結させることを
特徴とする請求項１または請求項２記載の低熱膨張セラ
ミックスの製造方法。3. Eucryptite 50 to 95% by volume, and α-, while controlling each manufacturing process so that the content of Fe 2 O 3 in the ceramics is 0.05% by weight or less.
SiC, β-SiC, Si 3 N 4 , TiB 2 , ZrB 2 , W
One or more compounds selected from C, TiC and ZrN 5
The method for producing a low thermal expansion ceramics according to claim 1 or 2, wherein a molded body made of 50% by volume is sintered at a temperature of 1100 to 1550 ° C in a vacuum or an inert gas atmosphere.
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| JP2007076949A (en) * | 2005-09-14 | 2007-03-29 | Taiheiyo Cement Corp | Black low resistance ceramic and member for semiconductor manufacturing device |
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| JPS5232596A (en) * | 1975-09-09 | 1977-03-11 | Tdk Corp | Conductive composite ceramics |
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| JPH10294264A (en) * | 1997-04-21 | 1998-11-04 | Hitachi Ltd | Electron beam lithography device |
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| JP2007076949A (en) * | 2005-09-14 | 2007-03-29 | Taiheiyo Cement Corp | Black low resistance ceramic and member for semiconductor manufacturing device |
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