JP2012162452A - Method for producing porous body - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 32
- 239000002184 metal Substances 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 15
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 239000011856 silicon-based particle Substances 0.000 claims abstract description 8
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 abstract description 50
- 229910052710 silicon Inorganic materials 0.000 description 23
- 239000010703 silicon Substances 0.000 description 23
- 238000010438 heat treatment Methods 0.000 description 10
- 235000012431 wafers Nutrition 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 239000011521 glass Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Ceramic Products (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Container, Conveyance, Adherence, Positioning, Of Wafer (AREA)
Abstract
Description
本発明は、半導体製造装置や液晶パネルをはじめとするフラットパネルディスプレイ製造装置などに使用される露光装置のようにパーティクルの発生が問題となる工程を必要とする各産業分野に関わる。 The present invention relates to various industrial fields that require a process in which generation of particles becomes a problem, such as an exposure apparatus used in a flat panel display manufacturing apparatus such as a semiconductor manufacturing apparatus and a liquid crystal panel.
セラミックス多孔体は耐熱性や耐蝕性に優れていることから半導体製造装置や液晶製造装置内のフィルター、雰囲気ガス等や洗浄液等をウエハやガラス基板等に供給するための給気部材や給液部材、およびウエハやガラス基板の吸着装置の吸着板等に使用されている。吸着装置としてはアルミニウムやステンレスなどの金属素材に溝や穴を開け、そこから吸引するものも多くある。 The ceramic porous body is excellent in heat resistance and corrosion resistance, so air supply members and liquid supply members for supplying filters, atmospheric gases, cleaning liquids, etc. in semiconductor manufacturing equipment and liquid crystal manufacturing equipment to wafers, glass substrates, etc. And a suction plate of a suction device for a wafer or a glass substrate. There are many suction devices that make grooves or holes in a metal material such as aluminum or stainless steel, and suck from the holes.
しかし、近年、ウエハや基板ガラスの大型化、薄型化に伴い、溝や穴などの特定部位から吸引する場合、被吸着物であるウエハや基板ガラスが変形し、高精度の吸着が出来ないことや、吸着力が不足するなどの問題が発生する。そのため、吸着装置として全面吸着することができる多孔体が多く用いられている。なかでも、ＳｉＣはＳｉウエハとの熱膨張率差が少ないことからＳｉウエハの搬送装置などに多く使用されており、吸着装置以外でのＳｉＣを用いた多孔体の活用も広がっている。 However, in recent years, when wafers and substrate glass are becoming larger and thinner, when sucked from specific parts such as grooves and holes, the wafer or substrate glass that is the object to be adsorbed is deformed and high-precision suction cannot be performed. In addition, problems such as insufficient suction force occur. Therefore, many porous bodies that can be adsorbed on the entire surface are used as adsorption devices. Especially, since SiC has a small difference in thermal expansion coefficient from the Si wafer, it is widely used in Si wafer transfer devices and the like, and the use of porous materials using SiC other than the adsorption device is also spreading.
このような多孔体に関する技術が種々提案されている。例えば、ＳｉＣ粉末に、金属シリコン粉末とフェノールなどの有機物を添加し、それらを反応させてＳｉＣ化することによるＳｉＣ粒子間を接合するものや発泡剤をいれるものなどがある。多孔体の強度は通常の緻密体より低く、そのため粒子の脱粒も起こりやすくなっている。また、残留しているカーボンなどによりパーティクルが多く発生するという問題点がある。 Various techniques relating to such a porous body have been proposed. For example, there are those that add metallic silicon powder and an organic substance such as phenol to SiC powder, react them to form SiC, and join SiC particles, and those that contain a foaming agent. The strength of the porous body is lower than that of a normal dense body, and therefore, the particles are easily shed. In addition, there is a problem that many particles are generated due to remaining carbon or the like.
骨材となる耐火性粒子と金属珪素とを含む多孔体が開示されている（特許文献１参照）。この多孔体は、耐火性粒子原料に、金属珪素と有機バインダーを添加し混合及び混練して得られた坏土を成形し、得られた成形体を仮焼して成形体中の有機バインダーを除去した後、本焼成する製造方法により得られる。この方法によれば、バインダーを除去しているので、残留カーボンによるパーティクルの発生を抑制できることが期待される。 A porous body containing refractory particles and metal silicon as an aggregate is disclosed (see Patent Document 1). This porous body is formed into a refractory particle raw material by adding metal silicon and an organic binder, mixing and kneading, and molding the kneaded clay. The resulting molded body is calcined to form an organic binder in the molded body. After removal, it is obtained by a production method in which firing is performed. According to this method, since the binder is removed, it is expected that generation of particles due to residual carbon can be suppressed.
しかしながら、本発明者の検討によれば、バインダーを除去しても、パーティクルの発生を十分に抑制することはできなかった。したがって、このような多孔体を半導体製造装置等の部材として用いると、ウエハやガラス基板にパーティクルが付着し、処理精度の低下を招く。 However, according to the study by the present inventor, even if the binder is removed, the generation of particles cannot be sufficiently suppressed. Therefore, when such a porous body is used as a member of a semiconductor manufacturing apparatus or the like, particles adhere to the wafer or glass substrate, resulting in a decrease in processing accuracy.
具体的には、給気部材や給液部材では、供給する気体や液体にパーティクルが紛れ込む場合があり、また、吸着装置でも直接接触するのでパーティクルがウエハ及びガラス基板に転移する場合があった。特に近年、半導体製造装置やフラットパネルディスプレイ製造装置の分野では、処理精度の高度化が著しく、より低パーティクル性の多孔体が望まれていた。 Specifically, in the air supply member or the liquid supply member, particles may be mixed into the supplied gas or liquid, and in some cases, the particles may be transferred to the wafer and the glass substrate because they are in direct contact with the adsorption device. In particular, in recent years, in the field of semiconductor manufacturing apparatuses and flat panel display manufacturing apparatuses, the processing accuracy has been remarkably advanced, and a porous body having a lower particle property has been desired.
パーティクルの発生源として残留カーボンの脱粒及びＳｉＣの脱粒があげられる。残留カーボンとしては、ＳｉＣ多孔体の接合材として使用されているフェノールなどバインダーの有機物が起因と考えられる。上述のように、通常、ＳｉＣの多孔体を作製する場合、カーボン源及び金属シリコンを添加し、これらを反応させてＳｉＣ化させることによりＳｉＣの粒子同士を接合させる。 Particle generation sources include residual carbon degranulation and SiC degranulation. It is considered that the residual carbon is caused by an organic substance such as phenol used as a bonding material for the SiC porous body. As described above, when producing a SiC porous body, normally, a carbon source and metal silicon are added, and these are reacted to form SiC, thereby joining SiC particles together.
このとき、すべてのカーボンがＳｉＣ化せず、一部が微細な残留カーボンとして残るため、これがパーティクルとなってしまう。残留カーボンについては、本焼成後に、有機溶剤等により洗浄することにより、ある程度除去することができる。しかし、完全に除去することは困難なので、できるだけ減らすことが好ましい。 At this time, all of the carbon is not converted to SiC, and a part of the carbon remains as fine residual carbon, which becomes particles. The residual carbon can be removed to some extent by washing with an organic solvent after the main firing. However, since it is difficult to remove completely, it is preferable to reduce as much as possible.
したがって、特許文献１に記載された発明によれば、カーボンを除去しているのでパーティクルを低減できることが期待されたが、十分に低減することはできなかった。そこで、パーティクル成分を調べたところ、カーボンは低減されているものの、ＳｉＣの脱粒が著しい。 Therefore, according to the invention described in Patent Document 1, it is expected that particles can be reduced because carbon is removed, but it cannot be sufficiently reduced. Therefore, when the particle component was examined, SiC was degranulated although carbon was reduced.
ここで、通常、ＳｉＣには遊離炭素が含まれており、遊離炭素は、バインダーの除去温度である１５０℃から７００℃では、除去することはできない。したがって、特許文献１に記載された発明のように、１４００℃以上に加熱して金属シリコンを軟化させて結合させる場合、カーボンとの反応性が高まるため、ＳｉＣに含まれる遊離炭素と反応して、微細なＳｉＣが生成する。これが、パーティクル源となったと考えられる。 Here, normally, free carbon is contained in SiC, and free carbon cannot be removed at a binder removal temperature of 150 ° C. to 700 ° C. Therefore, when the metal silicon is softened and bonded by heating to 1400 ° C. or more as in the invention described in Patent Document 1, the reactivity with carbon increases, so it reacts with free carbon contained in SiC. Fine SiC is generated. This is considered to be the particle source.
そこで、本発明は、パーティクルの発生個数の低減化が図られている多孔体の製造方法を提供することを解決課題とする。 Therefore, an object of the present invention is to provide a method for manufacturing a porous body in which the number of generated particles is reduced.
本発明者は、熱処理温度を下げることによりパーティクル発生量の少ない多孔体が得られることを知見した。 The present inventor has found that a porous body with a small amount of generated particles can be obtained by lowering the heat treatment temperature.
当該知見に基づく本発明の多孔体の製造方法は、１００重量部のＳｉＣ粉末と、５重量部以下のカーボン粉末または５重量部以下のカーボンを含む有機系バインダーと、２０重量部以上の金属シリコン粉末との混合粉末をプレス成形して成形体とする工程と、前記成形体を非酸化雰囲気中、１２００〜１３５０［℃］で熱処理することにより金属シリコンの粒子同士をネッキングさせる工程を含むことを特徴とする。 The method for producing a porous body of the present invention based on the above knowledge includes: 100 parts by weight of SiC powder, 5 parts by weight or less of carbon powder or 5 parts by weight or less of carbon-based organic binder, and 20 parts by weight or more of metallic silicon. Including a step of press-molding a mixed powder with the powder to form a molded body, and a step of necking the metal silicon particles by heat-treating the molded body at 1200 to 1350 [° C.] in a non-oxidizing atmosphere. Features.
熱処理温が１２００〜１３５０［℃］の温度範囲で実行されるので、金属シリコンのカーボンとの反応によるＳｉＣ化が防止され、かつ、金属シリコンの粒子同士のネッキングが促進される。また、熱処理雰囲気が非酸化雰囲気であるため、金属シリコンの表面にネッキングを阻害する酸化膜は生じない。 Since the heat treatment temperature is executed in a temperature range of 1200 to 1350 [° C.], the formation of SiC due to the reaction of metal silicon with carbon is prevented, and the necking of metal silicon particles is promoted. Moreover, since the heat treatment atmosphere is a non-oxidizing atmosphere, an oxide film that inhibits necking does not occur on the surface of the metal silicon.
したがって、金属シリコンの粒子同士が強固に結合した多孔体が得られる。金属シリコンのネッキングを進行させることにより金属シリコン粒子間の距離が小さくなり、ＳｉＣ粉末についても強固に締め付けられるため、脱粒を防ぐことができる。金属シリコンとＳｉＣ粉末とは反応しないと考えられるので、ＳｉＣ粉末の固定が問題となるが、金属シリコンの粒子同士のネッキングにより、ＳｉＣ粉末についても強固に締め付けられるため脱粒を防ぐことができる。ここで、有機系バインダーに含まれるカーボン量は、残留炭素量（コンラドソン法；ＪＩＳＫ２２７０）である。 Therefore, a porous body in which metallic silicon particles are firmly bonded to each other is obtained. By proceeding with the necking of the metal silicon, the distance between the metal silicon particles is reduced, and the SiC powder is also firmly clamped, so that the degranulation can be prevented. Since it is considered that the metal silicon and the SiC powder do not react with each other, the fixing of the SiC powder becomes a problem. However, since the SiC powder is firmly clamped by the necking of the particles of the metal silicon, the degranulation can be prevented. Here, the amount of carbon contained in the organic binder is the amount of residual carbon (Conradson method; JISK2270).
多孔体の原料である混合粉末におけるカーボンの含有量は、ＳｉＣ粉末１００重量部に対して５重量部以下であることが望ましい。カーボンが多いと、それ自体がパーティクル源となりやすいためであり、また、金属シリコンのネッキングを阻害するおそれがあるためである。また、混合粉末におけるカーボンの含有量は、ＳｉＣ粉末１００重量部に対して１重量部以上であることが望ましい。それ以下の添加量では本焼成前の成形体の作製が困難である。さらに金属シリコンによるネッキングが発生するまで、成形体を保持できなくなる。 The carbon content in the mixed powder, which is a raw material for the porous body, is desirably 5 parts by weight or less with respect to 100 parts by weight of the SiC powder. This is because if the amount of carbon is large, the carbon itself tends to be a particle source, and the necking of metal silicon may be hindered. Further, the carbon content in the mixed powder is desirably 1 part by weight or more with respect to 100 parts by weight of the SiC powder. If the addition amount is less than that, it is difficult to produce a molded body before the main firing. Further, the molded body cannot be held until necking with metallic silicon occurs.
多孔体の原料である混合粉末における金属シリコンの含有量は、ＳｉＣ粉末１００重量部に対して２０重量部以上であることが望ましい。金属シリコンの含有量が２０重量部に満たないと、多孔体全体の強度が低下するため好ましくない。また、金属シリコンの添加量の上限は６０重量部以下が望ましい。６０重量部よりも多く添加すると金属シリコンのネッキングにより、気孔率の制御が困難になる。 The content of metallic silicon in the mixed powder that is a raw material of the porous body is desirably 20 parts by weight or more with respect to 100 parts by weight of the SiC powder. If the content of metal silicon is less than 20 parts by weight, the strength of the entire porous body is lowered, which is not preferable. The upper limit of the amount of metal silicon added is preferably 60 parts by weight or less. If it is added in an amount of more than 60 parts by weight, it becomes difficult to control the porosity due to the necking of the metal silicon.
上述のように、金属シリコンの粒子同士がネッキングした構造とすることにより、パーティクルの発生が抑えられ、半導体製造装置及びフラットパネルディスプレイ製造装置に好適な多孔体を提供することができる。 As described above, by forming a structure in which metal silicon particles are necked, generation of particles can be suppressed, and a porous body suitable for a semiconductor manufacturing apparatus and a flat panel display manufacturing apparatus can be provided.
ＳｉＣ粉末としては平均粒径（Ｄ５０）が２０〜２００［μｍ］で、純度は９９［％］以上のものを使用する。平均粒径が２０［μｍ］より小さいと多孔体として十分な気孔径が確保できない。また、平均粒径が２００［μｍ］より大きいと粒子の表面積が大きいため、多孔体としての十分な強度が確保できない。また、純度については９８［％］以上であれば十分であり、市販の研磨材程度の純度で十分である。なお、ここで言う平均粒径（Ｄ５０）は、レーザ回折／散乱式粒子径分布測定装置（ＬＡ−９２０、堀場製作所（登録商標）製）を用いた測定値である。 A SiC powder having an average particle diameter (D50) of 20 to 200 [μm] and a purity of 99 [%] or more is used. When the average particle diameter is smaller than 20 [μm], a sufficient pore diameter as a porous body cannot be secured. Moreover, since the surface area of particle | grains is large when an average particle diameter is larger than 200 [micrometers], sufficient intensity | strength as a porous body cannot be ensured. Further, the purity is sufficient if it is 98 [%] or more, and a purity of about a commercially available abrasive is sufficient. In addition, the average particle diameter (D50) said here is a measured value using the laser diffraction / scattering type | formula particle size distribution measuring apparatus (LA-920, Horiba, Ltd. product (trademark)).
金属シリコンとしては平均粒径（Ｄ５０）が１０〜５０［μｍ］で純度は９９．９［％］以上のものを使用する。平均粒径が１０［μｍ］より小さい金属シリコンを使用すると表面に酸化膜が多く形成されている可能性が高く、熱処理の段階で酸化膜の影響により多孔体の強度を発現するために必要なネッキングが発生しない。また、平均粒径が５０［μｍ］よりも大きいと金属シリコンの分散に偏りが生じ、多孔体の強度が低下する。純度については、純度の低い金属シリコンを使用すると融点が低下するため、１２００〜１３５０［℃］程度の温度で熔解し、カーボンと反応する恐れがある。 Metallic silicon having an average particle diameter (D50) of 10 to 50 [μm] and a purity of 99.9 [%] or more is used. When metal silicon having an average particle size of less than 10 [μm] is used, there is a high possibility that a large amount of oxide film is formed on the surface, and it is necessary to develop the strength of the porous body due to the influence of the oxide film at the stage of heat treatment. Necking does not occur. On the other hand, when the average particle size is larger than 50 [μm], the dispersion of the metal silicon is biased and the strength of the porous body is lowered. Regarding the purity, since the melting point is lowered when metal silicon having a low purity is used, there is a possibility that it melts at a temperature of about 1200 to 1350 [° C.] and reacts with carbon.
カーボンとしては有機系のバインダーであれば液体でも粉末状のものでも構わない。ただし、高温での強度を考慮するとフェノール系のバインダーが望ましい。バインダーの残留炭素率（カーボン量）としては、４０〜６０重量部のものが混合粉末の成形に適している。 Carbon may be liquid or powder as long as it is an organic binder. However, considering the strength at high temperature, a phenolic binder is desirable. As the residual carbon ratio (carbon amount) of the binder, 40 to 60 parts by weight is suitable for forming the mixed powder.
混合粉末の成形方法は、公知の方法が採用できる。例えば、ＣＩＰ、プレス成形、押し出し成形等が適用できる。添加するバインダーによっては、成形体の強度を高めるために熱を加えても良い。 A known method can be adopted as a method for forming the mixed powder. For example, CIP, press molding, extrusion molding, etc. can be applied. Depending on the binder to be added, heat may be applied to increase the strength of the molded body.
金属シリコンをネッキングさせるための熱処理の雰囲気は、非酸化雰囲気が望ましい。具体的には、真空中やＡｒ等の不活性ガス中で熱処理することができる。 The atmosphere of the heat treatment for necking the metal silicon is preferably a non-oxidizing atmosphere. Specifically, heat treatment can be performed in a vacuum or an inert gas such as Ar.
本発明の多孔体は、気孔径が１０［μｍ］以上とすることが好ましい。１０［μｍ］未満では通風抵抗が大きく、フィルターとして使用する場合、好ましくない。また、上限については使用上の規定はないが、使用するＳｉＣ粉末の粒径などから１００［μｍ］以上の平均気孔径は多孔体の強度上、作製が困難である。 The porous body of the present invention preferably has a pore diameter of 10 [μm] or more. If it is less than 10 [μm], the ventilation resistance is large, which is not preferable when used as a filter. Moreover, although there is no restriction | limiting in use about an upper limit, preparation of the average pore diameter of 100 [micrometers] or more is difficult on the intensity | strength of a porous body from the particle size of the SiC powder to be used.
また、気孔率は、３０〜６０［％］であることが好ましい。この範囲の気孔率ならばフィルターなどとして使用する際の通風抵抗が最適である。気孔率が６０％より大きいと多孔体の強度が低下するという問題が発生する。 Moreover, it is preferable that a porosity is 30-60 [%]. If the porosity is within this range, the ventilation resistance when used as a filter or the like is optimal. If the porosity is larger than 60%, there arises a problem that the strength of the porous body is lowered.
以下、本発明の実施例を比較例とともに具体的に挙げ、本発明をより詳細に説明する。
［実施例１〜８、比較例１〜３］
市販のＳｉＣ粉末（粒径（Ｄ５０）１３５［μｍ］、純度９９［％］）、Ｓｉ粉末（粒径（Ｄ５０）４５［μｍ］、純度９９．９［％］）及びフェノール粉末（ノボラック型、残留炭素率５０重量部）を表１に示されている割合で混合し、１時間にわたり乾式混合する。その後、２０［ｋｇ／ｃｍ2］の圧力をかけながら１５０［℃］で１時間にわたり熱プレスを行った。熱プレス後、１２時間−１５０℃で硬化処理を行い、その後、表1の温度で熱処理（Ａｒ雰囲気）を行った。こうして得られた多孔体をパーティクルを測定するために□３０［ｍｍ］×ｔ３［ｍｍ］形状に加工した。加工後の洗浄はメタノールによる超音波洗浄（４０［ｋＨｚ］）を１５分間行った後、炭化水素系洗剤に３０分間浸漬、超純水に１０分間浸漬した。さらに超純水による超音波洗浄（４０［ｋＨｚ］）を１０分間にわたって行い、最後に超純水でシャワーを行った。その後、乾燥した後、測定を行った。
EXAMPLES Hereinafter, the Example of this invention is specifically given with a comparative example, and this invention is demonstrated in detail.
[Examples 1-8, Comparative Examples 1-3]
Commercially available SiC powder (particle size (D50) 135 [μm], purity 99 [%]), Si powder (particle size (D50) 45 [μm], purity 99.9 [%]) and phenol powder (novolak type, Residual carbon ratio 50 parts by weight) is mixed in the proportions shown in Table 1 and dry mixed for 1 hour. Thereafter, hot pressing was performed at 150 [° C.] for 1 hour while applying a pressure of 20 [kg / cm 2 ]. After hot pressing, a curing treatment was performed at −150 ° C. for 12 hours, and then a heat treatment (Ar atmosphere) was performed at the temperature shown in Table 1. The porous body thus obtained was processed into a shape of □ 30 [mm] × t3 [mm] in order to measure particles. After the processing, ultrasonic cleaning with methanol (40 [kHz]) was performed for 15 minutes, followed by immersion in a hydrocarbon-based detergent for 30 minutes and immersion in ultrapure water for 10 minutes. Furthermore, ultrasonic cleaning with ultrapure water (40 [kHz]) was performed for 10 minutes, and finally a shower was performed with ultrapure water. Then, after drying, measurement was performed.
パーティクルの発生個数の測定はリオン（登録商標）社製のＫＣ−２４を用いた。窒素ガスを、多孔体を介して吸引し、吸引したガスに含まれるパーティクルの発生個数を測定した。測定用の気体は液体窒素から取り出した窒素を使用し、窒素を満たした容器の出口に多孔体を取り付け、この多孔体と測定器から伸びているφ１０［ｍｍ］の吸引部を接続して、更に測定器の計測部分に接続した。パーティクル測定器の吸引流量は２８［ｌ／ｍｉｎ］とした。測定したパーティクルの粒子径は０．５［μｍ］以上で、１０分間測定しパーティクルの量をカウントした。なお、ブランクのパーティクル数は平均で１０個以下であった。パーティクルの測定結果を表1に示す。なお、気孔率はアルキメデス法で測定した。
［比較例４］
上記実施例と同様に成形したものを、熱処理において、７００［℃］まで大気中にて加熱し、バインダー起因のカーボンを除去した後に、Ａｒ雰囲気で加熱した。その他の工程は、上記実施例と同様に行った。
For the measurement of the number of generated particles, KC-24 manufactured by Rion (registered trademark) was used. Nitrogen gas was sucked through the porous body, and the number of generated particles contained in the sucked gas was measured. The measurement gas uses nitrogen extracted from liquid nitrogen, attaches a porous body to the outlet of the container filled with nitrogen, connects this porous body and a suction part of φ10 [mm] extending from the measuring instrument, Furthermore, it connected to the measurement part of the measuring instrument. The suction flow rate of the particle measuring device was 28 [l / min]. The measured particle diameter was 0.5 [μm] or more and measured for 10 minutes to count the amount of particles. The number of blank particles was 10 or less on average. Table 1 shows the particle measurement results. The porosity was measured by the Archimedes method.
[Comparative Example 4]
In the heat treatment, the material molded in the same manner as in the above example was heated to 700 [° C.] in the air to remove carbon derived from the binder, and then heated in an Ar atmosphere. Other steps were performed in the same manner as in the above example.
表１から明らかなように、すべての実施例でパーティクル数が５０個以下であった。比較例１〜３では、実施例と比べて、パーティクル数は著しく多くなった。バインダーを除去した比較例４でもパーティクル数が多かった。したがって、１００重量部のＳｉＣ粉末に対して、５重量部以下のカーボン及び２０重量部以上の金属シリコンとからなり、１２００〜１３５０℃の低温で熱処理して得られる多孔体により、パーティクルを低減できることが分かった。光学顕微鏡で、本発明の多孔体（実施例１〜８）を観察したところ、金属シリコン粒子は溶融せずに隣接する粒子とネッキングしており、ＳｉＣ粉末粒子との濡れは見られなかった。 As is apparent from Table 1, the number of particles was 50 or less in all examples. In Comparative Examples 1 to 3, the number of particles was remarkably increased compared to the Examples. In Comparative Example 4 where the binder was removed, the number of particles was large. Therefore, particles can be reduced by a porous body obtained by heat treatment at a low temperature of 1200 to 1350 ° C., comprising 5 parts by weight or less of carbon and 20 parts by weight or more of metal silicon with respect to 100 parts by weight of SiC powder. I understood. When the porous body of the present invention (Examples 1 to 8) was observed with an optical microscope, the metal silicon particles were not melted but were adjacent to the adjacent particles, and wetting with the SiC powder particles was not observed.
以上より、本発明の多孔体は、金属シリコンのネッキング構造を有しており、パーティクルの発生が少なく、半導体製造装置及びフラットパネルディスプレイ製造装置に好適に使用できることが示された。 From the above, it has been shown that the porous body of the present invention has a metal silicon necking structure, generates less particles, and can be suitably used for semiconductor manufacturing apparatuses and flat panel display manufacturing apparatuses.
Claims (1)
前記成形体を非酸化雰囲気中、１２００〜１３５０［℃］で熱処理することにより金属シリコンの粒子同士をネッキングさせる工程を含むことを特徴とする多孔体の製造方法。 A mixed powder of 100 parts by weight of SiC powder, 5 parts by weight or less of carbon powder or organic binder containing 5 parts by weight or less of carbon, and 20 parts by weight or more of metal silicon powder is press-molded to form a compact. Process,
The manufacturing method of the porous body characterized by including the process of necking the metal silicon particles by heat-processing the said molded object at 1200-1350 [degreeC] in non-oxidizing atmosphere.
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