JP2005314157A - Silicon carbide sintered compact and semiconductor using the same, and member for liquid crystal-manufacturing apparatus - Google Patents
Silicon carbide sintered compact and semiconductor using the same, and member for liquid crystal-manufacturing apparatus Download PDFInfo
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Abstract
Description
本発明は、高緻密な炭化珪素焼結体およびそれを用いた半導体および液晶製造装置用部材に関する。 The present invention relates to a high-density silicon carbide sintered body and a semiconductor and liquid crystal manufacturing apparatus member using the same.
精密光学機器等に使用されるミラーは、主として、ガラスやルビー、サファイア等の単結晶セラミックスが使用されている。しかしながら、ガラスを用いたミラーは強度が弱く、割れやすいという問題がある。また、ルビーやサファイア等の単結晶は、製品が高額になるという問題がある。 Mirrors used in precision optical equipment and the like are mainly made of single crystal ceramics such as glass, ruby, and sapphire. However, the mirror using glass has a problem that the strength is weak and the glass is easily broken. In addition, single crystals such as ruby and sapphire have a problem that the product is expensive.
このような問題を解決するために、近年、ミラー等の光学部品に多結晶セラミックスが用いられてきている（例えば、特許文献１参照）。しかしながら、多結晶セラミックスでは、表面を鏡面研磨した際にそのセラミックス自体が有する空孔（ポア）が研磨面に残存し、この鏡面研磨面に金属を蒸着した面の反射率が十分満足するものが得られないという問題がある。
本発明はこのような事情に鑑みてなされたものであり、空孔が極めて少ない高緻密な炭化珪素焼結体を提供することを目的とする。また、本発明は、このような炭化珪素焼結体を用いた半導体および液晶製造装置用部材を提供することを目的とする。 This invention is made | formed in view of such a situation, and it aims at providing the highly precise | minute silicon carbide sintered compact with very few void | holes. Another object of the present invention is to provide a semiconductor and liquid crystal manufacturing apparatus member using such a silicon carbide sintered body.
本発明によれば、焼結助剤として、アルミニウムおよび／またはアルミニウム化合物と、ホウ素および／またはホウ素化合物と、炭素および／または炭化可能な化合物と、を含む炭化珪素焼結体であって、
相対密度が９８％以上であり、その鏡面研磨面の中心線平均粗さ（Ｒａ）が１５ｎｍ以下であることを特徴とする炭化珪素焼結体、が提供される。
According to the present invention, there is provided a silicon carbide sintered body containing, as a sintering aid, aluminum and / or an aluminum compound, boron and / or a boron compound, and carbon and / or a carbonizable compound,
A silicon carbide sintered body characterized in that the relative density is 98% or more and the center line average roughness (Ra) of the mirror-polished surface is 15 nm or less.
この炭化珪素焼結体は、炭化珪素粉末に、アルミニウム換算量で０．１〜２．５％のアルミニウムまたはアルミニウム化合物と、ホウ素換算量で０．１〜２．０％のホウ素またはホウ素化合物と、炭素換算量で１．０〜４．０％の炭素または炭化可能な化合物を添加して混合し、これを成形して得られた成形体を、少なくともＡｌ８Ｂ４Ｃ７を含む液相によって焼結するように１７５０〜２１００℃での不活性ガス雰囲気において焼成したものであることが好ましい。ここで、この焼成は０．１ＭＰａ以上の加圧雰囲気で行われることが好ましい。また、炭化珪素焼結体は、前記成形体を前記焼成条件で焼成した後、さらに１７５０〜２１００℃で０．１ＭＰａ以上の不活性ガス雰囲気下で熱処理することにより得られたものであることも好ましい。 This silicon carbide sintered body is obtained by adding 0.1 to 2.5% aluminum or aluminum compound in terms of aluminum and 0.1 to 2.0% boron or boron compound in terms of boron to silicon carbide powder. A liquid phase containing at least Al 8 B 4 C 7 is obtained by adding and mixing 1.0 to 4.0% carbon or a carbonizable compound in terms of carbon and mixing the mixture. It is preferable that it is fired in an inert gas atmosphere at 1750 to 2100 ° C. so as to sinter. Here, this firing is preferably performed in a pressurized atmosphere of 0.1 MPa or more. In addition, the silicon carbide sintered body may be obtained by firing the molded body under the firing conditions and then performing a heat treatment at 1750 to 2100 ° C. in an inert gas atmosphere of 0.1 MPa or more. preferable.
本発明によれば、上記炭化珪素焼結体からなることを特徴とする半導体および液晶製造装置用部材、が提供される。
この半導体および液晶製造装置用部材の好適な例としては、炭化珪素焼結体の所定の面が鏡面研磨処理され、その鏡面研磨面に反射率が７５％以上となる金属膜が設けられているミラー部材が挙げられる。
According to the present invention, there is provided a member for a semiconductor and liquid crystal manufacturing apparatus, characterized by comprising the silicon carbide sintered body.
As a preferable example of the semiconductor and liquid crystal manufacturing apparatus member, a predetermined surface of the silicon carbide sintered body is mirror-polished, and a metal film having a reflectance of 75% or more is provided on the mirror-polished surface. A mirror member is mentioned.
本発明に係る炭化珪素焼結体は、空孔が極めて少なく、高緻密で表面粗さが小さいために、反射率の高い金属膜を形成することが容易となる。 Since the silicon carbide sintered body according to the present invention has very few pores, is highly dense, and has a small surface roughness, it is easy to form a metal film having a high reflectance.
以下、本発明について詳細に説明する。本発明に係る炭化珪素焼結体は、炭化珪素粉末に、焼結助剤としてアルミニウムおよび／またはアルミニウム化合物（つまり、アルミニウムとアルミニウム化合物の一方か両方）と、ホウ素および／またはホウ素化合物と、炭素および／または炭化可能な化合物とが含まれる。これは、製造プロセスの焼結段階において、Ａｌ８Ｂ４Ｃ７組成を主成分とする液相を高温で発生させて、炭化珪素の焼結を促進させるためである。 Hereinafter, the present invention will be described in detail. The silicon carbide sintered body according to the present invention includes silicon carbide powder, aluminum and / or aluminum compound (that is, one or both of aluminum and aluminum compound), boron and / or boron compound, and carbon as a sintering aid. And / or carbonizable compounds. This is to promote the sintering of silicon carbide by generating a liquid phase mainly composed of Al 8 B 4 C 7 at a high temperature in the sintering stage of the manufacturing process.
アルミニウム化合物としてはＡｌ３Ｃ４、ＡｌＢ２、ＡｌＢ１２が、ホウ素化合物としてはＢ４Ｃが、炭素としては黒鉛粉末が、炭化可能な化合物としてはフェノール樹脂等の各種樹脂材料が、それぞれ好適に用いられる。 As the aluminum compound, Al 3 C 4 , AlB 2 , and AlB 12 are preferable, B 4 C as the boron compound, graphite powder as the carbon, and various resin materials such as a phenol resin as the carbonizable compound, respectively. Used.
これら焼結助剤の添加量は、アルミニウム換算量で０．１〜２．５％、ホウ素換算量で０．１〜２．０％、炭素換算量で１．０〜４．０％とすることが好ましい。焼結助剤がこの範囲よりも少ない場合は、焼結中にＡｌ８Ｂ４Ｃ７組成を主成分とする液相が生成せず、緻密な焼結体を得ることが困難である。また焼結助剤がこの範囲よりも多い場合は、炭化珪素粒子が過度に粗大化するために、鏡面研磨面の中心線平均粗さ（Ｒａ）を１５ｎｍ以下とすることが困難となる。 The addition amount of these sintering aids is 0.1 to 2.5% in terms of aluminum, 0.1 to 2.0% in terms of boron, and 1.0 to 4.0% in terms of carbon. It is preferable. When the sintering aid is less than this range, a liquid phase mainly composed of the Al 8 B 4 C 7 composition is not generated during sintering, and it is difficult to obtain a dense sintered body. When the sintering aid is larger than this range, the silicon carbide particles are excessively coarsened, so that it is difficult to set the center line average roughness (Ra) of the mirror-polished surface to 15 nm or less.
本発明に係る炭化珪素焼結体は、相対密度が９８％以上であり、その鏡面研磨面の中心線平均粗さ（Ｒａ）を１５ｎｍ以下とする。これにより、この鏡面研磨面に金属を蒸着して反射膜を形成した場合に、精密光学機器等に使用されるミラーとして好適な光学的特性である７５％以上という反射率を得ることが容易となる。 The silicon carbide sintered body according to the present invention has a relative density of 98% or more, and the center line average roughness (Ra) of the mirror-polished surface is 15 nm or less. As a result, when a reflective film is formed by depositing metal on this mirror-polished surface, it is easy to obtain a reflectance of 75% or more, which is an optical characteristic suitable as a mirror used in precision optical equipment and the like. Become.
本発明に係る炭化珪素焼結体の製造方法は、次の通りである。最初に、炭化珪素粉末に、アルミニウム換算量で０．１〜２．５％のアルミニウムまたはアルミニウム化合物と、ホウ素換算量で０．１〜２．０％のホウ素またはホウ素化合物と、炭素換算量で１．０〜４．０％の炭素または炭化可能な化合物を添加して混合し、これを公知の成形方法、例えば、一軸プレス成形やＣＩＰ成形により所定の形状に成形する。 The manufacturing method of the silicon carbide sintered body according to the present invention is as follows. First, in silicon carbide powder, 0.1 to 2.5% aluminum or aluminum compound in terms of aluminum, 0.1 to 2.0% boron or boron compound in terms of boron, and carbon equivalent 1.0 to 4.0% of carbon or a carbonizable compound is added and mixed, and this is molded into a predetermined shape by a known molding method such as uniaxial press molding or CIP molding.
こうして作製した成形体を焼成処理する。その方法としては、（ａ）少なくともＡｌ８Ｂ４Ｃ７を含む液相によって焼結するように１７５０〜２１００℃での不活性ガス雰囲気において焼成する方法、（ｂ）前記（ａ）の焼成を０．１ＭＰａ以上の加圧雰囲気で行う方法、（ｃ）前記（ａ）により得られた炭化珪素焼結体をさらに１７５０〜２１００℃で０．１ＭＰａ以上の不活性ガス雰囲気下で熱処理する方法、が好適に用いられる。なお、前記（ａ）は、所謂、常圧焼結法である。前記（ｂ）の処理方法を、以下、「直接加圧熱処理法」といい、前記（ｃ）の処理方法を、以下、「間接加圧熱処理法」ということとする。 The molded body thus produced is fired. The method includes (a) a method of firing in an inert gas atmosphere at 1750 to 2100 ° C. so as to sinter in a liquid phase containing at least Al 8 B 4 C 7 , and (b) the firing of (a). A method of performing in a pressurized atmosphere of 0.1 MPa or more, (c) a method of further heat-treating the silicon carbide sintered body obtained by the above (a) at 1750 to 2100 ° C. in an inert gas atmosphere of 0.1 MPa or more, Are preferably used. Note that (a) is a so-called atmospheric pressure sintering method. Hereinafter, the treatment method (b) is referred to as “direct pressure heat treatment method”, and the treatment method (c) is hereinafter referred to as “indirect pressure heat treatment method”.
炭化珪素の焼成温度を１７５０〜２１００℃としたのは、１７５０℃より低い場合には緻密な炭化珪素焼結体が得られ難く、一方、２１００℃より高い場合には炭化珪素粒子が粗大化し過ぎてしまうために、後に鏡面研磨を行う際に中心線平均粗さ（Ｒａ）を１５ｎｍ以下とすることが困難になるためである。また、焼結工程は、所定の密度が得られる限りにおいて、常圧焼結法を用いることが製造コスト面では有利である。直接加圧熱処理法や間接加圧熱処理法では、常圧焼結法と比較して製造コストは高くなるが、より高緻密の焼結体を得られるという利点がある。なお、直接加圧熱処理法と間接加圧熱処理法では、不活性ガス雰囲気の圧力を０．１ＰＭａ未満とすると、気孔を消滅させる効果が得られ難い。 The reason why the firing temperature of silicon carbide is 1750 to 2100 ° C. is that when it is lower than 1750 ° C., it is difficult to obtain a dense silicon carbide sintered body, whereas when it is higher than 2100 ° C., silicon carbide particles are too coarse. Therefore, when mirror polishing is performed later, it is difficult to make the center line average roughness (Ra) 15 nm or less. In addition, as long as a predetermined density is obtained, it is advantageous in terms of production cost to use the atmospheric pressure sintering method in the sintering process. The direct pressure heat treatment method and the indirect pressure heat treatment method have a manufacturing cost higher than that of the normal pressure sintering method, but have an advantage that a denser sintered body can be obtained. In the direct pressure heat treatment method and the indirect pressure heat treatment method, if the pressure of the inert gas atmosphere is less than 0.1 PMa, it is difficult to obtain the effect of eliminating the pores.
次に、本発明を実施例および比較例により具体的に説明する。
（試料製造方法）
原料の炭化珪素粉末に、下記表１に示した各種の焼結助剤と、成形助剤（バインダー）としてのポリビニルブチラールと、２−プロパノールを所定量添加し、混合した。次いで、こうして得られたスラリーをスプレードライヤーで顆粒とし、得られた顆粒をＣＩＰ成形した。得られた成形体を、非酸化物セラミックスの焼結に好適に用いられる炭素抵抗加熱炉を用い、アルゴン雰囲気下、表１に示した温度条件で焼結した。
Next, the present invention will be specifically described with reference to examples and comparative examples.
(Sample manufacturing method)
A predetermined amount of various sintering aids shown in Table 1 below, polyvinyl butyral as a molding aid (binder), and 2-propanol were added to the raw material silicon carbide powder and mixed. Next, the slurry thus obtained was granulated with a spray dryer, and the obtained granule was CIP-molded. The obtained molded body was sintered under a temperature condition shown in Table 1 in an argon atmosphere using a carbon resistance heating furnace suitably used for sintering non-oxide ceramics.
なお、一般的に炭化珪素粉末は不純物として酸化珪素を含んでおり、この酸化珪素は炭化珪素の焼結を阻害する。そこで、酸化珪素による焼結阻害を防止するために、１４００℃から１６００℃までの間は真空雰囲気として数時間保持することにより、酸化珪素を顆粒中のＣと反応させる。その後、１６００℃以上では再びアルゴン雰囲気に戻す。 In general, silicon carbide powder contains silicon oxide as an impurity, and this silicon oxide inhibits the sintering of silicon carbide. Therefore, in order to prevent sintering inhibition due to silicon oxide, silicon oxide is reacted with C in the granules by maintaining a vacuum atmosphere for several hours between 1400 ° C. and 1600 ° C. Thereafter, the atmosphere is returned to the argon atmosphere again at 1600 ° C. or higher.
（評価方法）
得られた焼結体の相対密度はアルキメデス法により、焼結体中のＡｌ８Ｂ４Ｃ７相の同定はＸＲＤにより、鏡面研磨面の中心線平均粗さ（Ｒａ）は接触式表面粗さ計により、それぞれ評価した。また、焼結体の鏡面研磨面にＡｌ膜を蒸着し、その面に６３３ｎｍの波長の光をあててその反射率を測定した。
(Evaluation methods)
The relative density of the obtained sintered body was determined by the Archimedes method, the Al 8 B 4 C 7 phase in the sintered body was identified by XRD, and the center line average roughness (Ra) of the mirror-polished surface was the contact surface roughness. Each was evaluated by the total. Further, an Al film was deposited on the mirror polished surface of the sintered body, and the reflectance was measured by applying light having a wavelength of 633 nm to the surface.
（試験結果）
試験結果を表１に並記する。表１から明らかなように、実施例１〜７では７５％以上の良好な反射率を示し、特に直接加圧熱処理法または間接加圧熱処理法により作製された実施例４〜７では、高い相対密度および８５％以上の高い反射率を示した。
(Test results)
The test results are listed in Table 1. As is apparent from Table 1, Examples 1 to 7 show a good reflectance of 75% or more, and in Examples 4 to 7 produced by the direct pressure heat treatment method or the indirect pressure heat treatment method, in particular, a high relative The density and high reflectivity of 85% or more were shown.
これに対して比較例１〜６では、緻密な焼結体を得ることができなかった。比較例１〜３では焼結体中にＡｌ８Ｂ４Ｃ７が認められなかったことから、アルミニウム成分、ホウ素成分、カーボン成分のいずれかの添加量が少ないために、焼結中にＡｌ８Ｂ４Ｃ７が生成せず、緻密化が進まなかったものと考えられる。一方、比較例４〜６では、アルミニウム成分、ホウ素成分、カーボン成分のいずれかの添加量が必要以上であるために、炭化珪素粒子の粗大化が過度に進行し、このために鏡面研磨面の中心線平均粗さ（Ｒａ）を１５ｎｍ以下に加工することができず、７５％より低い反射率を示した。 In contrast, in Comparative Examples 1 to 6, a dense sintered body could not be obtained. In Comparative Examples 1 to 3, since Al 8 B 4 C 7 was not observed in the sintered body, the amount of any of the aluminum component, boron component, and carbon component was small, so that Al 8 B It is considered that B 4 C 7 was not generated and densification did not proceed. On the other hand, in Comparative Examples 4 to 6, since the addition amount of any one of the aluminum component, boron component, and carbon component is more than necessary, the coarsening of the silicon carbide particles proceeds excessively. The center line average roughness (Ra) could not be processed to 15 nm or less, and the reflectance was lower than 75%.
比較例７では焼成温度が低いために、比較例９では加圧熱処理温度が低いために、ともに緻密化が不十分であった。比較例８，１０，１１では９８％以上の相対密度が得られたが、比較例８では焼成温度が高いために、比較例１０，１１では加圧熱処理温度が高いために、ともに炭化珪素粒子が粗大化し過ぎ、このために鏡面研磨面の中心線平均粗さ（Ｒａ）を１５ｎｍ以下に加工することができず、７５％より低い反射率を示した。 In Comparative Example 7, the firing temperature was low, and in Comparative Example 9, the pressure heat treatment temperature was low. In Comparative Examples 8, 10, and 11, a relative density of 98% or more was obtained. However, in Comparative Example 8, the firing temperature was high, and in Comparative Examples 10 and 11, the pressure heat treatment temperature was high. Thus, the center line average roughness (Ra) of the mirror-polished surface could not be processed to 15 nm or less, and the reflectance was lower than 75%.
本発明は、露光装置におけるステージ位置測定用ミラー等、精密光学機器用のミラーに好適である。 The present invention is suitable for a mirror for precision optical equipment such as a stage position measuring mirror in an exposure apparatus.
Claims (6)
相対密度が９８％以上であり、その鏡面研磨面の中心線平均粗さ（Ｒａ）が１５ｎｍ以下であることを特徴とする炭化珪素焼結体。 A silicon carbide sintered body containing, as a sintering aid, aluminum and / or an aluminum compound, boron and / or a boron compound, and carbon and / or a carbonizable compound,
A silicon carbide sintered body having a relative density of 98% or more and a center line average roughness (Ra) of the mirror-polished surface of 15 nm or less.
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| JPH09268062A (en) * | 1996-03-29 | 1997-10-14 | Nippon Steel Corp | Silicon carbide sintered compact and its production |
| JPH11292631A (en) * | 1998-04-16 | 1999-10-26 | Natl Inst For Res In Inorganic Materials | Low-temperature sintering of silicon carbide powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05246764A (en) * | 1991-12-19 | 1993-09-24 | Nippon Steel Corp | High-purity dense silicon carbide sintered body, substrate for reflection mirror and production thereof |
| JPH06300907A (en) * | 1993-04-16 | 1994-10-28 | Nippon Steel Corp | Parts for optical purpose and x-ray formed by using silicon carbide sintered compact and their production |
| JPH09268062A (en) * | 1996-03-29 | 1997-10-14 | Nippon Steel Corp | Silicon carbide sintered compact and its production |
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