JP4231638B2 - Control method of volume resistivity of low thermal expansion ceramics - Google Patents
Control method of volume resistivity of low thermal expansion ceramics Download PDFInfo
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- JP4231638B2 JP4231638B2 JP2001209143A JP2001209143A JP4231638B2 JP 4231638 B2 JP4231638 B2 JP 4231638B2 JP 2001209143 A JP2001209143 A JP 2001209143A JP 2001209143 A JP2001209143 A JP 2001209143A JP 4231638 B2 JP4231638 B2 JP 4231638B2
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- silicon carbide
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- thermal expansion
- volume resistivity
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- 239000000919 ceramic Substances 0.000 title claims description 18
- 238000000034 method Methods 0.000 title claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 28
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 22
- 239000002131 composite material Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 229910000174 eucryptite Inorganic materials 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000013329 compounding Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は、低熱膨張高剛性セラミックスに関するもので、さらに詳しくは、半導体製造装置、特に静電チャックに用いられる低熱膨張高剛性セラミックスに関するものである。
【０００２】
【従来の技術】
従来、半導体の製造工程におけるシリコンウェハの指示固定には、静電吸着力を応用した静電チャックが広く用いられている。ここで静電吸着力とは、支持台（チャックとも呼ぶ。）とこれに接触させたウェハとの間に高電圧を印加した時に発生する静電気による吸着力であり、チャックの素材としては、１×１０10Ω・ｃｍ程度の体積抵抗率を有することが好ましく、多くの場合、窒化アルミニウムが用いられている。
【０００３】
【発明が解決しようとする課題】
半導体部品は、その内部や外部に回路が設けられているが、製造工程において温度変化が生じると、製造装置を構成する各部品が熱膨張または収縮し、回路の配線にずれが生じるという課題がある。特に近年は、あらゆる電気製品が軽薄短小化の傾向にあるため半導体部品の回路パターンも微細になってきており、わずかな温度変化によっても歩留まりが低下することが問題となってきている。
ここで、従来使用されている窒化アルミニウムの熱膨張係数は４×１０6／℃と大きいため、温度変化に大きく影響を受ける。そこで、室温における熱膨張係数が非常に小さい材料が求められてきている。
【０００４】
【課題を解決するための手段】
したがって、本出願人はこれまでにも、負の熱膨張係数を持つユークリプタイトとα型炭化珪素とを複合させることで２３℃近辺での熱膨張係数が０．０×１０-6／℃、体積抵抗率が１０12Ω・ｃｍ程度である材料を開発し提案している。またさらに、炭化珪素としてβ型を用いることで体積抵抗率を１×１０6Ω・ｃｍ程度に低下させることができることを見出した。
つぎに、α型とβ型の炭化珪素を同時添加する方法を試みたところ、α型とβ型の比を変えることで、熱膨張係数およびヤング率を維持したまま、複合セラミックスを任意の体積抵抗率に制御出来ることを見出し、本発明を完成したものである。
【０００５】
すなわち、本発明は上記課題を解決するために鋭意検討して完成したものであり、その要旨は、ユークリプタイト７０〜９５体積％と炭化珪素５〜３０体積％とからなる複合セラミックスにおいて、前記炭化珪素の結晶形態の配合割合がα型／β型の体積配合比で６０／４０から３／９７の範囲であることを特徴とする低熱膨張高剛性セラミックスである。
【０００６】
【発明の実施の形態】
本発明では、ユークリプタイト７０〜９５体積％と炭化珪素５〜３０体積％とからなる複合セラミックスにおいて、前記炭化珪素の結晶形態の配合割合がα型／β型の体積配合比で６０／４０から３／９７の範囲であることを特徴とする低熱膨張高剛性セラミックスを提案している。
ここで、前記炭化珪素の結晶形態の配合割合をα型／β型の体積配合比で６０／４０から３／９７の範囲とした理由は、α型／β型の体積配合比で６０／４０より大きいと体積抵抗率がα型の炭化珪素のみを複合させた場合とほとんど変わらず、α型／β型の体積配合比が３／９７より小さいとβ型の炭化珪素のみを複合させた場合とほとんど変わらないからである。
【０００７】
ここで、体積抵抗率を従来の窒化アルミニウムと同程度の１×１０10Ω・ｃｍとするためには、炭化珪素の結晶形態の配合割合をα型／β型の体積配合比で４０／６０から２０／８０の範囲とすることが特に好ましい。
【０００８】
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
市販のユークリプタイト粉末とα型炭化珪素粉末およびβ型炭化珪素粉末を出発原料として、焼結後の複合セラミックスのユークリプタイトが８０ｖｏｌ％でα型炭化珪素粉末およびβ型炭化珪素粉末の合量が２０ｖｏｌ％となるようにし、さらに炭化珪素粉末のα型／β型の体積配合比が１００／０から０／１００の範囲となるように種々の配合割合の出発原料を配合し、これをボールミルで粉砕・混合した。乾燥させた後にＣＩＰ成形し、窒素雰囲気において１３５０℃で焼成し、複合セラミックスを得た。得られた複合セラミックスを２．０ｍｍの厚さに加工し、体積抵抗率測定用試験片とした。
【０００９】
（２）評価
次に、試験片の表裏面にＡｇ電極を形成し、三端子法によって体積抵抗率を測定した。印加電圧は５００Ｖとし、室温における体積抵抗率を求めた。得られた結果を図１にまとめて示した。（ここで図中の縦軸は体積抵抗率を表示したものであるが、縦軸の例えば、１．００Ｅ＋１３とは１０の冪指数を略号化したものであり、１．００×１０13と同義である。また、横軸は炭化珪素のα型／β型の体積配合比で、１００／０とはα型の炭化珪素のみを配合したものを示し、また、０／１００とはβ型の炭化珪素のみを配合したものを示している。）
また、別途、各試験片の熱膨張係数とヤング率を公知の方法で評価したが、いずれの試験片も熱膨張係数は０．０×１０-6／℃と低熱膨張であり、ヤング率は１５０ＧＰａ以上と高剛性であった。すなわち、本発明に係わる複合セラミックスの熱膨張係数とヤング率の値は、炭化珪素のα型／β型の体積配合比にはほとんど影響されなかった。
【００１０】
図１から明らかなように、炭化珪素の結晶形態の配合割合をα型／β型の体積配合比で４０／６０から２０／８０の範囲で変えることで、熱膨張係数を０．０×１０-6／℃、ヤング率を１５０ＧＰａ以上に維持したまま、体積抵抗率を１．００×１０12〜１．００×１０6の範囲で所望の値に変化させることができることが分かった。さらに、体積抵抗率を従来の窒化アルミニウムと同程度の１×１０10Ω・ｃｍ程度とするためには、炭化珪素の結晶形態の配合割合をα型／β型の体積配合比で４０／６０から２０／８０の範囲とすることが好ましいことも分かった。
【００１１】
【発明の効果】
以上説明したように、本発明によれば、低熱膨張高剛性という特長を維持したまま体積抵抗率の値を任意に制御可能であり、特に、従来の窒化アルミニウムに替えて本発明による複合セラミックスを静電チャックとして用いた場合には、温度変化に起因する歩留まり低下を格段に抑制できるという効果がある。
【図面の簡単な説明】
【図１】本発明に係わる複合セラミックスの体積抵抗率と複合セラミックスの炭化珪素のα型／β型の体積配合割合を示した図である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a low thermal expansion high rigidity ceramic, and more particularly to a semiconductor manufacturing apparatus, particularly a low thermal expansion high rigidity ceramic used for an electrostatic chuck.
[0002]
[Prior art]
2. Description of the Related Art Conventionally, electrostatic chucks using electrostatic attraction force have been widely used for indicating and fixing silicon wafers in semiconductor manufacturing processes. Here, the electrostatic attracting force is an attracting force due to static electricity generated when a high voltage is applied between a support base (also referred to as a chuck) and a wafer in contact with the support. It preferably has a volume resistivity of about × 10 10 Ω · cm, and in many cases, aluminum nitride is used.
[0003]
[Problems to be solved by the invention]
Semiconductor components are provided with circuits inside and outside. However, when temperature changes occur in the manufacturing process, there is a problem in that each component of the manufacturing apparatus thermally expands or contracts, causing a shift in circuit wiring. is there. In particular, in recent years, since every electric product has a tendency to be lighter, thinner, and smaller, circuit patterns of semiconductor components have become finer, and it has become a problem that the yield decreases even with a slight temperature change.
Here, since the thermal expansion coefficient of conventionally used aluminum nitride is as large as 4 × 10 6 / ° C., it is greatly affected by temperature change. Therefore, a material having a very small coefficient of thermal expansion at room temperature has been demanded.
[0004]
[Means for Solving the Problems]
Therefore, the present applicant has so far made a composite of eucryptite having a negative thermal expansion coefficient and α-type silicon carbide to have a thermal expansion coefficient of about 0.0 × 10 −6 / ° C. near 23 ° C. A material having a volume resistivity of about 10 12 Ω · cm has been developed and proposed. Furthermore, it has been found that the volume resistivity can be reduced to about 1 × 10 6 Ω · cm by using β-type as silicon carbide.
Next, an attempt was made to add α-type and β-type silicon carbide at the same time. By changing the ratio of α-type and β-type, the composite ceramic can be added to any volume while maintaining the thermal expansion coefficient and Young's modulus. The inventors have found that the resistivity can be controlled and completed the present invention.
[0005]
That is, the present invention has been completed through intensive studies in order to solve the above-mentioned problems, and the gist of the present invention is a composite ceramic material composed of 70 to 95% by volume of eucryptite and 5 to 30% by volume of silicon carbide. It is a low thermal expansion and high rigidity ceramic characterized in that the mixing ratio of the crystal form of silicon carbide is in the range of 60/40 to 3/97 in the volume ratio of α type / β type.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
In the present invention, in a composite ceramic composed of 70 to 95% by volume of eucryptite and 5 to 30% by volume of silicon carbide, the compounding ratio of the crystalline form of the silicon carbide is 60/40 in terms of an α type / β type volume mixing ratio. To 3/97, a low thermal expansion and high rigidity ceramic is proposed.
Here, the reason why the mixing ratio of the crystal form of the silicon carbide is in the range of 60/40 to 3/97 in the volume ratio of α type / β type is that the volume ratio of α type / β type is 60/40. When larger, the volume resistivity is almost the same as when only α-type silicon carbide is combined, and when α-type / β-type volume blend ratio is less than 3/97, only β-type silicon carbide is combined Because it is almost the same.
[0007]
Here, in order to set the volume resistivity to 1 × 10 10 Ω · cm, which is about the same as that of conventional aluminum nitride, the proportion of silicon carbide in the crystal form is 40/60 in terms of the α-type / β-type volume mixture ratio. To 20/80 is particularly preferable.
[0008]
Hereinafter, the present invention will be described in detail with reference to examples and comparative examples, but the present invention is not limited to the examples.
(1) Manufacturing method of composite ceramics Starting from commercially available eucryptite powder, α-type silicon carbide powder and β-type silicon carbide powder, α-type silicon carbide powder containing 80 vol% eucryptite of the composite ceramic after sintering And β-type silicon carbide powder so that the total amount is 20 vol%, and the α-type / β-type volume mixture ratio of the silicon carbide powder is in the range of 100/0 to 0/100. The starting materials were blended and pulverized and mixed with a ball mill. After drying, CIP molding was performed and firing was performed at 1350 ° C. in a nitrogen atmosphere to obtain a composite ceramic. The obtained composite ceramics was processed to a thickness of 2.0 mm to obtain a test piece for measuring volume resistivity.
[0009]
(2) Evaluation Next, Ag electrodes were formed on the front and back surfaces of the test piece, and the volume resistivity was measured by the three-terminal method. The applied voltage was 500 V, and the volume resistivity at room temperature was determined. The obtained results are summarized in FIG. (Here, the vertical axis in the figure represents the volume resistivity. For example, 1.00E + 13 on the vertical axis is an abbreviation of the power index of 10 and is synonymous with 1.00 × 10 13. The horizontal axis is the α / β type volume mixing ratio of silicon carbide, where 100/0 indicates only α type silicon carbide, and 0/100 indicates β type. (Only silicon carbide is blended.)
Separately, the thermal expansion coefficient and Young's modulus of each test piece were evaluated by a known method. All the test pieces have a low thermal expansion coefficient of 0.0 × 10 −6 / ° C., and the Young's modulus is The rigidity was as high as 150 GPa or more. That is, the values of the thermal expansion coefficient and the Young's modulus of the composite ceramic according to the present invention were hardly influenced by the α / β type volume mixing ratio of silicon carbide.
[0010]
As is apparent from FIG. 1, the thermal expansion coefficient is changed to 0.0 × 10 by changing the blending ratio of the silicon carbide crystal form in the range of 40/60 to 20/80 as the volume blending ratio of α type / β type. It was found that the volume resistivity can be changed to a desired value in the range of 1.00 × 10 12 to 1.00 × 10 6 while maintaining the −6 / ° C. and Young's modulus at 150 GPa or more. Furthermore, in order to set the volume resistivity to about 1 × 10 10 Ω · cm, which is the same as that of the conventional aluminum nitride, the mixing ratio of the silicon carbide crystal form is 40/60 in terms of the α type / β type volume mixing ratio. It was also found that it is preferable to set the range to 20/80.
[0011]
【The invention's effect】
As described above, according to the present invention, the value of volume resistivity can be arbitrarily controlled while maintaining the characteristics of low thermal expansion and high rigidity. In particular, the composite ceramic according to the present invention can be used in place of conventional aluminum nitride. When used as an electrostatic chuck, there is an effect that yield reduction due to temperature change can be remarkably suppressed.
[Brief description of the drawings]
FIG. 1 is a diagram showing the volume resistivity of a composite ceramic according to the present invention and the α / β type volume blending ratio of silicon carbide of the composite ceramic.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2001209143A JP4231638B2 (en) | 2001-07-10 | 2001-07-10 | Control method of volume resistivity of low thermal expansion ceramics |
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| JP2001209143A JP4231638B2 (en) | 2001-07-10 | 2001-07-10 | Control method of volume resistivity of low thermal expansion ceramics |
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| JP4231638B2 true JP4231638B2 (en) | 2009-03-04 |
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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 |
| ES2354099B1 (en) * | 2009-08-27 | 2012-01-19 | CONSEJO SUPERIOR DE INVESTIGACIONES CIENTÍFICAS (CSIC) (Titular al 66,66%) | PROCEDURE FOR OBTAINING CERAMIC COMPOUNDS, AND MATERIAL OBTAINABLE BY SUCH PROCEDURE. |
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