JP2000327461A - Regenerated graphite material coated with silicon carbide - Google Patents
Regenerated graphite material coated with silicon carbideInfo
- Publication number
- JP2000327461A JP2000327461A JP34981399A JP34981399A JP2000327461A JP 2000327461 A JP2000327461 A JP 2000327461A JP 34981399 A JP34981399 A JP 34981399A JP 34981399 A JP34981399 A JP 34981399A JP 2000327461 A JP2000327461 A JP 2000327461A
- Authority
- JP
- Japan
- Prior art keywords
- silicon carbide
- coated
- defect
- layer
- carbide layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Container, Conveyance, Adherence, Positioning, Of Wafer (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、炭化ケイ素が被覆
された黒鉛基材において、炭化ケイ素表面のピンホール
や欠け等の欠陥を補修して再利用可能とする再生炭化ケ
イ素被覆黒鉛材とその再生法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a reclaimed silicon carbide-coated graphite material which repairs defects such as pinholes and chips on the surface of the silicon carbide and makes it reusable. Reproduction method.
【０００２】[0002]
【従来の技術】炭化ケイ素被覆黒鉛材は、高温でのシリ
コンとの耐反応性や、不純物含有量が非常に少ないとい
う特性を持っており、半導体製造工程において、エピタ
キシャル成長用サセプターや、引き上げ装置用部材等と
して広く利用されている。2. Description of the Related Art Graphite materials coated with silicon carbide have characteristics of high resistance to silicon at high temperatures and very low impurity content. In a semiconductor manufacturing process, susceptors for epitaxial growth and susceptors for pulling devices are used. Widely used as members and the like.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、炭化ケ
イ素被覆黒鉛材をエピタキシャル成長用サセプターや、
引き上げ装置用部材として繰り返し使用していると、黒
鉛基材と炭化ケイ素間に存在していた不純物と反応した
り、また、黒鉛基材表面に存在していた欠陥等のため、
炭化ケイ素被覆層の表面にピンホール状の欠陥が発生
し、黒鉛基材が露出する場合がある。また、各装置への
設置作業中や、運搬中等に何らかの原因で、炭化ケイ素
被覆層の一部が欠けてしまって、前記ピンホールと同様
に黒鉛基材が露出してしまう場合がある。このような場
合、半導体製造工程に使用すると、黒鉛基材より不純物
ガスが発生して、製品に悪影響を及ぼしてしまう。その
ため、黒鉛基材が少しでも露出してしまった場合は、使
用せずに廃棄処分されていた。However, a graphite material coated with silicon carbide is used as a susceptor for epitaxial growth,
When repeatedly used as a member for a lifting device, it reacts with impurities present between the graphite substrate and silicon carbide, and, due to defects etc. existing on the surface of the graphite substrate,
Pinhole-shaped defects may be generated on the surface of the silicon carbide coating layer, exposing the graphite substrate. Further, during installation work to each device, during transportation, or the like, for some reason, a part of the silicon carbide coating layer may be chipped and the graphite substrate may be exposed similarly to the pinhole. In such a case, when used in a semiconductor manufacturing process, an impurity gas is generated from the graphite base material, which adversely affects the product. Therefore, if the graphite substrate is exposed at all, it has been disposed of without being used.
【０００４】また、ピンホール等は不純物等が原因とな
っていることが多く、これら不純物を除去して炭化ケイ
素を被覆しなければ、また、ピンホールの発生原因にな
るとともに、場合によっては、炭化ケイ素被覆後、その
表面に黒い斑紋がでる場合がある。[0004] In addition, pinholes and the like are often caused by impurities and the like. Unless these impurities are removed and coated with silicon carbide, pinholes and the like may be generated. After coating with silicon carbide, black spots may appear on the surface.
【０００５】そこで、本発明は前記課題を解決するため
になされたものであり、ピンホールや欠け等の欠陥によ
り黒鉛基材が露出した炭化ケイ素被覆黒鉛材に再度炭化
ケイ素で被覆しても、炭化ケイ素の表面に黒い斑紋等が
現れず、再利用可能となる再生炭化ケイ素被覆黒鉛材と
その再生法を提供することを目的とする。Accordingly, the present invention has been made to solve the above-mentioned problems, and the present invention is directed to a silicon carbide-coated graphite material in which a graphite base material is exposed due to defects such as pinholes and chips, and is again coated with silicon carbide. It is an object of the present invention to provide a recycled silicon carbide-coated graphite material which does not show black marks or the like on the surface of silicon carbide and can be reused, and a method for regenerating the same.
【０００６】[0006]
【課題を解決するための手段】前記課題を解決するため
の本発明の再生炭化ケイ素被覆黒鉛材は、黒鉛基材の表
面に第１炭化ケイ素層が被覆され、前記第１炭化ケイ素
層の欠陥が炭素材で埋められ、前記第１炭化ケイ素層の
表面に第２炭化ケイ素層が被覆されたものである。ま
た、前記欠陥のうち少なくとも１つが前記第１炭化ケイ
素層を貫通するものである。また、前記第１炭化ケイ素
層と前記第２炭化ケイ素層との間に不純物を介在させな
いものである。また、前記不純物が、ブラスト処理、酸
洗浄処理、熱処理、ハロゲン処理のいずれか若しくは２
以上を組み合わせて除去されたものである。また、前記
欠陥の大きさが、０．３ｍｍ以上であるものである。According to the present invention, there is provided a recycled silicon carbide-coated graphite material according to the present invention, wherein a surface of a graphite substrate is coated with a first silicon carbide layer, and the first silicon carbide layer has defects. Is filled with a carbon material, and the surface of the first silicon carbide layer is coated with a second silicon carbide layer. Further, at least one of the defects penetrates the first silicon carbide layer. Further, no impurities are interposed between the first silicon carbide layer and the second silicon carbide layer. Further, the impurity is any one of blast treatment, acid cleaning treatment, heat treatment, and halogen treatment or 2
These are removed by combining the above. Further, the size of the defect is 0.3 mm or more.
【０００７】このように、本発明の再生炭化ケイ素被覆
黒鉛材は、先に形成され、半導体製造工程におけるエピ
タキシャル成長用サセプター等として使用され、発生し
た第１炭化ケイ素層の欠陥の不純物を除去して、その欠
陥に炭素材を埋めて、欠陥部分の表面を平面とし、再度
炭化ケイ素を被覆し、平滑な面の第２炭化ケイ素層を形
成し、エピタキシャル成長用サセプター等として再度利
用できるようにしたものである。As described above, the recycled silicon carbide-coated graphite material of the present invention is formed first, is used as a susceptor for epitaxial growth in a semiconductor manufacturing process, etc., and removes generated impurities of defects of the first silicon carbide layer. The defect is buried with a carbon material, the surface of the defective portion is made flat, the silicon carbide is coated again, a second silicon carbide layer having a smooth surface is formed, and it can be reused as a susceptor or the like for epitaxial growth. It is.
【０００８】本発明で使用される黒鉛基材は一般的な製
法で作製された高純度等方性黒鉛が好ましい。特に、嵩
密度１．７ｇ／ｃｍ3 以上、水銀圧入法による平均気孔
径半径が５０μｍ以下、熱膨張係数が４．０×１０-6／
℃以上、不純物含有量が灰分量で１０ｐｐｍ以下である
ことが好ましい。また、前記黒鉛基材に強化材として炭
素繊維が含まれているものであっても構わない。The graphite substrate used in the present invention is preferably high-purity isotropic graphite produced by a general production method. In particular, the bulk density is 1.7 g / cm 3 or more, the average pore diameter radius by a mercury intrusion method is 50 μm or less, and the thermal expansion coefficient is 4.0 × 10 −6 /.
It is preferable that the impurity content is not less than 10 ° C. and the ash content is not more than 10 ppm. Further, the graphite base material may contain carbon fiber as a reinforcing material.
【０００９】この黒鉛基材に被覆された第１炭化ケイ素
被覆層は、ＣＶＤ（Ｃｈｅｍｉｃａｌ Ｖａｐｏｒ Ｄ
ｅｐｏｓｉｔｉｏｎ）法により形成されていることが好
ましい。ここで、第１炭化ケイ素被覆層は、黒鉛基材に
被覆された炭化ケイ素被覆層をいい、本発明において
は、半導体製造工程時に使用される時の、最外表面層に
被覆された炭化ケイ素を表す。したがって、この炭化ケ
イ素層の下側で、黒鉛基材との間に別の層が介在してい
る場合をも含んでいる。この炭化ケイ素被覆層は、厚み
が３０μｍ〜１４０μｍであることが好ましい。３０μ
ｍより薄い場合は、ピンホール等の欠陥が発生した場合
に、直ちに黒鉛基材に該欠陥が至ってしまうからであ
る。また、１４０μｍ以上であると、繰り返し使用され
ることにより受ける熱履歴によって容易に剥離してしま
うためである。The first silicon carbide coating layer coated on the graphite substrate is formed by CVD (Chemical Vapor D).
It is preferably formed by an evaporation method. Here, the first silicon carbide coating layer refers to a silicon carbide coating layer coated on a graphite substrate, and in the present invention, when used in a semiconductor manufacturing process, the silicon carbide coating layer coated on the outermost surface layer Represents Therefore, the case where another layer is interposed between the silicon carbide layer and the graphite base under the silicon carbide layer is also included. This silicon carbide coating layer preferably has a thickness of 30 μm to 140 μm. 30μ
When the thickness is smaller than m, when a defect such as a pinhole occurs, the defect immediately reaches the graphite base material. On the other hand, if the thickness is 140 μm or more, the film is easily peeled off due to the heat history received by repeated use.
【００１０】第１炭化ケイ素被覆層が被覆された状態
で、通常は、半導体製造工程におけるエピタキシャル成
長用サセプター等として使用することが可能となる。し
かしながら、前述したように、この第１炭化ケイ素被覆
層とその下側に存在する層との界面に、不純物や黒鉛基
材表面にピンホール等の欠陥が存在していた場合、また
は、第１炭化ケイ素被覆層の表面に不純物が付着した場
合等に、繰り返し熱履歴を受けると、これら欠陥によ
り、第１炭化ケイ素被覆層表面に、ピンホールやクラッ
ク等の欠陥が発生する。これら第１炭化ケイ素被覆層の
表面に発生する欠陥は、時にはこの第１炭化ケイ素被覆
層を貫通し、第１炭化ケイ素被覆層の下部層や黒鉛基材
に至る場合もある。この場合、下部の層や黒鉛基材より
不純物ガスが発生し、製造過程にある製品に悪影響を及
ぼしてしまう。また、炭化ケイ素は脆性材料であるた
め、僅かな衝撃で欠けたり、クラックが発生したりす
る。そのため、装置への設置途中や、運搬途中に何らか
の原因で、衝撃を受けることがあり、この第１炭化ケイ
素被覆層に欠けやクラックなどの欠陥が発生することも
ある。これら欠陥が前記ピンホール等の欠陥と同様に第
１炭化ケイ素被覆層を貫通して、第１炭化ケイ素被覆層
の下部層や黒鉛基材に到達してしまうこともある。この
ため、これら欠陥が発生した時点で、それが実際の製造
工程に使用前であっても廃棄処分されていた。With the first silicon carbide coating layer coated, it can usually be used as a susceptor for epitaxial growth in a semiconductor manufacturing process. However, as described above, when an impurity or a defect such as a pinhole is present on the graphite base material surface at the interface between the first silicon carbide coating layer and the layer existing therebelow, When a thermal history is repeatedly applied, for example, when impurities are attached to the surface of the silicon carbide coating layer, these defects cause defects such as pinholes and cracks on the surface of the first silicon carbide coating layer. Defects that occur on the surface of the first silicon carbide coating layer sometimes penetrate the first silicon carbide coating layer and reach the lower layer of the first silicon carbide coating layer or the graphite substrate. In this case, impurity gas is generated from the lower layer and the graphite base material, which has an adverse effect on the product in the manufacturing process. Further, since silicon carbide is a brittle material, it is chipped or cracked by a slight impact. For this reason, impact may occur for some reason during installation to the apparatus or during transportation, and defects such as chipping and cracks may occur in the first silicon carbide coating layer. These defects may penetrate the first silicon carbide coating layer and reach the lower layer of the first silicon carbide coating layer or the graphite substrate similarly to the defects such as the pinholes. Therefore, when these defects occur, they have been disposed of even before they are used in the actual manufacturing process.
【００１１】しかしながら、これら欠陥が大きすぎた
り、不純物が原因で発生した欠陥であったりすると、そ
の表面に再度炭化ケイ素を被覆しても、炭化ケイ素が被
覆されず、被覆されても、表面に黒い斑紋等が発生して
しまう。However, if these defects are too large or are defects caused by impurities, even if the surface is coated with silicon carbide again, silicon carbide is not coated, and even if the surface is coated, silicon carbide is not coated. Black spots and the like are generated.
【００１２】そこで、前記のように欠陥の発生した第１
炭化ケイ素被覆層を、ブラスト処理、酸洗浄処理、熱処
理、ハロゲン処理のいずれか１つ若しくは２つ以上を組
み合わせた処理を施し、表面に付着した不純物を除去す
ることが好ましい。ここで、ブラスト処理とは、金属粉
やセラミック粉を表面に高速でぶつけることによって表
面に付着した不純物を除去する処理をいい、酸洗浄処理
とは、フッ酸、フッ硝酸や、これらの混酸等により表面
を洗浄することをいい、熱処理とは、２０００℃以上の
還元雰囲気下における加熱処理をいい、ハロゲン処理と
は、塩素等を含むハロゲンガスによって表面を洗浄する
処理をいう。このような処理を施すことにより、エピタ
キシャル成長用サセプターとして使用され、その表面に
何らかの原因で付着した不純物を除去することができ
る。そして、これらの処理のいずれか１つ若しくは２つ
以上組み合わせて処理することにより、欠陥表面に付着
した不純物も除去することが可能となる。In view of the above, the first defect, as described above,
It is preferable that the silicon carbide coating layer is subjected to one or a combination of two or more of a blast treatment, an acid cleaning treatment, a heat treatment, and a halogen treatment to remove impurities attached to the surface. Here, blasting refers to a process of removing impurities attached to the surface by blasting metal powder or ceramic powder at high speed on the surface, and acid cleaning refers to hydrofluoric acid, hydrofluoric acid, or a mixed acid thereof. The heat treatment refers to a heat treatment in a reducing atmosphere at 2000 ° C. or higher, and the halogen treatment refers to a treatment for cleaning the surface with a halogen gas containing chlorine or the like. By performing such a treatment, impurities used as a susceptor for epitaxial growth and adhering to the surface for some reason can be removed. By performing one or a combination of two or more of these processes, it is possible to remove impurities attached to the defect surface.
【００１３】次に、この欠陥に、炭素材を充填して、欠
陥を埋めて平滑な面にすることが好ましい。ここで、使
用される炭素材は、硬化後に緻密になる、高純度で、粘
性の高い熱硬化性樹脂が好ましい。この熱硬化性樹脂と
しては、フェノール樹脂、エポキシ樹脂等が例示でき、
これらを単独若しくは１以上を組み合わせて使用するこ
とが好ましい。さらには、これら熱硬化性樹脂に黒鉛粉
末を添加したものを使用することも可能である。Next, it is preferable to fill the defect with a carbon material and fill the defect to make the surface smooth. Here, the carbon material used is preferably a high-purity, highly viscous thermosetting resin that becomes dense after curing. Examples of the thermosetting resin include a phenol resin and an epoxy resin.
It is preferable to use these alone or in combination of one or more. Furthermore, it is also possible to use those obtained by adding graphite powder to these thermosetting resins.
【００１４】これら炭素材は、第２炭化ケイ素層を形成
する際の加熱により炭化される。この炭素材の充填方法
は、特に限定されないが、先端をピン状に加工した炭素
棒の先端に、炭素材を付け、各欠陥に押し込むように充
填して、第１炭化ケイ素被覆層２と同一平面になるよう
に、高純度の炭素材からなる小片で、擦り合わせ、同一
平面を出すようにすることが好ましい。これによって、
第２炭化ケイ素被覆層を形成した場合に平滑な面とする
ことが可能となる。[0014] These carbon materials are carbonized by heating when forming the second silicon carbide layer. The method of filling the carbon material is not particularly limited, but a carbon material is attached to the tip of a carbon rod whose tip is processed into a pin shape, and the carbon material is filled so as to be pushed into each defect, and is the same as the first silicon carbide coating layer 2. It is preferable that small pieces made of a high-purity carbon material are rubbed so as to be flat, so that the same plane is obtained. by this,
When the second silicon carbide coating layer is formed, a smooth surface can be obtained.
【００１５】炭素材を欠陥に充填後、炭素材を硬化処理
することなく、この上に直接炭化ケイ素層をＣＶＤ法に
より被覆して、第２炭化ケイ素被覆層を形成することが
できる。また、欠陥が大きく、使用した炭素材が多い場
合は、第２炭化ケイ素被覆層をＣＶＤ処理により形成す
る前に、２００〜４００℃で熱処理を行いこの炭素材の
硬化処理を行うとともに、炭素材からの脱ガス処理を行
うことが好ましい。硬化処理後、炭素材の表面に気泡が
発生した場合等は、再度前記炭素材をその部分に充填
し、その表面に炭化ケイ素層をＣＶＤ法により形成し、
第２炭化ケイ素被覆層とすることができる。After filling the defect with the carbon material, a second silicon carbide coating layer can be formed by directly coating a silicon carbide layer on the carbon material by a CVD method without curing the carbon material. In addition, when the defect is large and a large amount of carbon material is used, before forming the second silicon carbide coating layer by the CVD process, a heat treatment is performed at 200 to 400 ° C. to cure the carbon material, Is preferably performed. After the curing treatment, when air bubbles are generated on the surface of the carbon material, the carbon material is filled in the portion again, and a silicon carbide layer is formed on the surface by a CVD method.
It can be a second silicon carbide coating layer.
【００１６】第１炭化ケイ素被覆層及び第２炭化ケイ素
被覆層を形成するＣＶＤ法に使用される原料ガスとして
は、ＳｉＣｌ4 とＣ3 Ｈ8 の混合ガスや、ＳｉＨ4 とＣ
3 Ｈ 8 の混合ガス等が例示できる。この原料ガスにキャ
リアーガスとして水素ガスを使用して、黒鉛基材温度１
０００〜１４００℃、常圧という条件で、ＣＶＤ処理を
行い、全面に炭化ケイ素層を被覆させる。First silicon carbide coating layer and second silicon carbide
As a source gas used in the CVD method for forming the coating layer
Is SiClFourAnd CThreeH8Mixed gas or SiHFourAnd C
ThreeH 8And the like. This source gas
Using hydrogen gas as the rear gas, graphite substrate temperature 1
Under the condition of 000-1400 ° C. and normal pressure, the CVD process
Then, the entire surface is coated with a silicon carbide layer.
【００１７】前記条件で形成される第２炭化ケイ素被覆
層は、厚みが２０μｍ〜１００μｍであることが好まし
い。１００μｍ以上であると、第１炭化ケイ素被覆層と
の界面で剥離が生じやすくなるため、厚みは、８０μｍ
以下、さらに好ましくは５０μｍ以下であることが好ま
しい。The second silicon carbide coating layer formed under the above conditions preferably has a thickness of 20 μm to 100 μm. When the thickness is 100 μm or more, separation easily occurs at the interface with the first silicon carbide coating layer.
The thickness is more preferably 50 μm or less.
【００１８】ところで、この欠陥の大きさＬ（図２参
照）が０．３ｍｍ未満の場合は、その表面の不純物を除
去し、該欠陥に炭素材を充填せずにＣＶＤ法により第２
炭化ケイ素層を被覆することで、第１炭化ケイ素被覆層
の表面の欠陥を塞ぐことが可能である。ここで、欠陥の
大きさＬは、ピンホールの場合はその外径を表してお
り、クラックの場合はその幅を表している。ところが、
これら欠陥の大きさが０．３ｍｍ以上の場合、炭素材を
欠陥に充填せずに、ＣＶＤ法で第２炭化ケイ素被覆層を
形成させると、図２に示すように欠陥５の外縁部分のみ
被覆され、欠陥５の内面から底部にかけては、炭化ケイ
素被覆層が形成されないこととなる。このように、欠陥
５の大きさＬが０．３ｍｍ以上の場合は、本発明のよう
に欠陥を予め埋め、その表面に炭化ケイ素被覆層を形成
することで、欠陥等によって使用が不能になった炭化ケ
イ素被覆黒鉛材の欠陥を補修することが可能となり、再
利用が可能となる。When the size L of the defect is less than 0.3 mm (see FIG. 2), impurities on the surface are removed, and the defect is not filled with a carbon material.
By covering the silicon carbide layer, defects on the surface of the first silicon carbide covering layer can be closed. Here, the size L of a defect represents the outer diameter of a pinhole, and the width of a crack. However,
When the size of these defects is 0.3 mm or more, if the second silicon carbide coating layer is formed by the CVD method without filling the defects with the carbon material, only the outer edge portions of the defects 5 are covered as shown in FIG. As a result, no silicon carbide coating layer is formed from the inner surface to the bottom of defect 5. As described above, when the size L of the defect 5 is 0.3 mm or more, the defect cannot be used due to the defect or the like by previously filling the defect and forming a silicon carbide coating layer on the surface as in the present invention. The defect of the silicon carbide-coated graphite material that has been repaired can be repaired and reused.
【００１９】以上のように、エピタキシャル成長用サセ
プターとして使用され、大きさが０．３ｍｍ以上の欠陥
や、黒鉛基材等に貫通するような欠陥が原因でライフエ
ンドとなったサセプターも、その表面の不純物を除去
し、欠陥を炭素材で埋めて、再度炭化ケイ素層を被覆す
ることでエピタキシャル成長用サセプターとして再利用
することが可能となる。また、欠け等により黒鉛が露出
した場合においても、本発明の方法で補修が可能とな
る。なお、エピタキシャル成長用サセプターのように、
ピンホール発生時期が予めわかっているような部材は、
ピンホールが発生する前に第１炭化ケイ素層表面の不純
物を任意の方法で除去し、第２炭化ケイ素層を被覆する
ことも有効である。As described above, a susceptor which is used as a susceptor for epitaxial growth and has a life end due to a defect having a size of 0.3 mm or more or a defect penetrating into a graphite substrate, etc. By removing impurities, filling defects with a carbon material, and coating the silicon carbide layer again, it becomes possible to reuse the silicon carbide layer as a susceptor for epitaxial growth. Further, even when graphite is exposed due to chipping or the like, repair can be performed by the method of the present invention. In addition, like the susceptor for epitaxial growth,
For members whose pinhole occurrence time is known in advance,
It is also effective to remove impurities on the surface of the first silicon carbide layer by any method before the generation of pinholes, and to cover the second silicon carbide layer.
【００２０】[0020]
【発明の実施形態】以下、本発明の実施形態例を図面を
参照しつつ具体的に説明する。Embodiments of the present invention will be specifically described below with reference to the drawings.
【００２１】図１には、本発明を適用した再生炭化ケイ
素被覆黒鉛材の一部断面概略図を示す。図において、１
は黒鉛基材、２は欠陥５が発生した第１炭化ケイ素被覆
層、３は再度被覆した第２炭化ケイ素層、４は欠陥５を
埋めた炭素材を示す。FIG. 1 is a schematic partial cross-sectional view of a recycled silicon carbide-coated graphite material to which the present invention is applied. In the figure, 1
Denotes a graphite substrate, 2 denotes a first silicon carbide coating layer in which defects 5 are generated, 3 denotes a second silicon carbide layer coated again, and 4 denotes a carbon material in which the defects 5 are buried.
【００２２】エピタキシャル成長用サセプターとして使
用し、その表面に何らかの原因で発生した大きさ０．３
ｍｍ以上の欠陥５が発生したサセプターの表面をブラス
ト処理する。ブラスト処理後、表面についたブラスト処
理に使用したセラミック粉末等を除去し、塩素ガスによ
って表面を洗浄する。洗浄後、表面の欠陥５に炭素材４
を充填する。炭素材４には、炭素化率の高いフェノール
樹脂を用い、先端を尖らせた高純度処理された黒鉛材に
より、欠陥５内に押し込むようにして充填する。欠陥５
に炭素材４を充填後、高純度の黒鉛材からなる小片で、
その表面を擦り合わせ、第１炭化ケイ素層２表面と同一
平面を出すようにする。次に、その表面にＳｉＣｌ4 と
Ｃ3 Ｈ8 の混合ガスを原料ガスとして、キャリアーガス
として水素ガスを使用して、１３００℃、１０１ｋＰａ
で、ＣＶＤ処理を行い、第２炭化ケイ素層３を５０μｍ
の厚みで形成した。第２炭化ケイ素層３の表面には、黒
い斑紋等は発生しなかった。また、エピタキシャル成長
用サセプターとして使用しても、シリコンウェハー上に
形成される結晶にも、異常が見られず、エピタキシャル
成長用サセプターとして再利用することが可能となっ
た。It is used as a susceptor for epitaxial growth and has a size of 0.3
The surface of the susceptor on which the defect 5 of not less than mm is blasted. After the blast treatment, the ceramic powder and the like used for the blast treatment on the surface are removed, and the surface is washed with chlorine gas. After cleaning, carbon material 4
Fill. The carbon material 4 is filled with a phenol resin having a high carbonization rate, and is pushed into the defect 5 with a graphite material having a sharpened tip and a high purity treatment. Defect 5
After filling carbon material 4 into small pieces made of high-purity graphite,
The surfaces are rubbed so as to be flush with the surface of first silicon carbide layer 2. Next, a mixed gas of SiCl 4 and C 3 H 8 was used as a source gas on the surface thereof, and a hydrogen gas was used as a carrier gas.
Then, the second silicon carbide layer 3 is subjected to a CVD process to a thickness of 50 μm.
Formed with a thickness of Black spots and the like did not occur on the surface of second silicon carbide layer 3. Further, even when used as a susceptor for epitaxial growth, no abnormality was found in the crystals formed on the silicon wafer, and the crystal could be reused as a susceptor for epitaxial growth.
【００２３】[0023]
【発明の効果】本発明によれば、炭化ケイ素被覆黒鉛材
の表面に発生したピンホールやクラック等の欠陥によっ
て使用が不能となったものを、その欠陥を補修して再度
利用することが可能となる。例えば、従来ピンホールに
よりライフエンドとなっていたエピタキシャル成長用サ
セプターの場合においても、その表面の不純物を除去
し、ピンホールを炭素材で埋めてその表面に炭化ケイ素
被覆層を再度形成させることで、表面に黒い斑紋等が発
生せず、再利用、すなわち再生させることが可能とな
り、サセプターの製造コストの大幅な削減が可能とな
る。また、使用前に何らかの原因で欠け等の欠陥で、黒
鉛が露出してしまった場合も、本発明により、補修して
利用することが可能となる。According to the present invention, it is possible to repair a defect that cannot be used due to a defect such as a pinhole or a crack generated on the surface of a silicon carbide-coated graphite material and repair the defect. Becomes For example, even in the case of a susceptor for epitaxial growth, which has conventionally been a life end due to a pinhole, removing impurities on the surface, filling the pinhole with a carbon material, and forming a silicon carbide coating layer on the surface again, Black spots and the like are not generated on the surface, so that the surface can be reused, that is, reproduced, and the production cost of the susceptor can be significantly reduced. Further, even if graphite is exposed due to a defect such as chipping for some reason before use, it can be repaired and used according to the present invention.
【図１】本発明による、再生炭化ケイ素被覆黒鉛材の一
部の断面概略図である。FIG. 1 is a schematic cross-sectional view of a part of a recycled silicon carbide-coated graphite material according to the present invention.
【図２】本発明における炭化ケイ素表面に発生する欠陥
の大きさを説明するための図である。FIG. 2 is a diagram for explaining the size of defects generated on the surface of silicon carbide in the present invention.
１ 黒鉛基材 ２ 第１炭化ケイ素被覆層 ３ 第２炭化ケイ素被覆層 ４ 炭素材 ５ 欠陥 Reference Signs List 1 graphite base material 2 first silicon carbide coating layer 3 second silicon carbide coating layer 4 carbon material 5 defect
Claims (9)
覆され、前記第１炭化ケイ素層の欠陥が炭素材で埋めら
れ、前記第１炭化ケイ素層の表面に第２炭化ケイ素層が
被覆された再生炭化ケイ素被覆黒鉛材。1. A surface of a graphite substrate is coated with a first silicon carbide layer, a defect of the first silicon carbide layer is filled with a carbon material, and a second silicon carbide layer is formed on a surface of the first silicon carbide layer. Graphite material coated with recycled silicon carbide.
１炭化ケイ素層を貫通するものである請求項１に記載の
再生炭化ケイ素被覆黒鉛材。2. The recycled silicon carbide-coated graphite material according to claim 1, wherein at least one of the defects penetrates the first silicon carbide layer.
イ素層との間に不純物を介在させない請求項１に記載の
再生炭化ケイ素被覆黒鉛材。3. The recycled silicon carbide-coated graphite material according to claim 1, wherein no impurities are interposed between the first silicon carbide layer and the second silicon carbide layer.
理、熱処理、ハロゲン処理のいずれか１つ若しくは２つ
以上を組み合わせて除去された請求項３に記載の再生炭
化ケイ素被覆黒鉛材。4. The recycled silicon carbide-coated graphite material according to claim 3, wherein said impurities have been removed by one or a combination of two or more of blast treatment, acid cleaning treatment, heat treatment, and halogen treatment.
ある請求項１乃至４のいずれかに記載の再生炭化ケイ素
被覆黒鉛材。5. The graphite material coated with recycled silicon carbide according to claim 1, wherein the size of the defect is 0.3 mm or more.
成長用サセプターとして適用される請求項１乃至５のい
ずれかに記載の再生炭化ケイ素被覆黒鉛材。6. The recycled silicon carbide-coated graphite material according to claim 1, which is used as a susceptor for epitaxial growth in a semiconductor manufacturing process.
鉛基材の、前記第１炭化ケイ素層の欠陥に、炭素前駆体
を埋め、その表面に第２炭化ケイ素層を被覆すると同時
に前記炭素前駆体を炭化する再生炭化ケイ素被覆黒鉛材
の再生法。7. A graphite substrate having a surface coated with a first silicon carbide layer, wherein a defect of the first silicon carbide layer is filled with a carbon precursor, and the surface of the graphite substrate is coated with a second silicon carbide layer. A method for recycling a recycled silicon carbide-coated graphite material that carbonizes a carbon precursor.
除去後、前記欠陥に炭素前駆体を埋め、その表面に第２
炭化ケイ素層を被覆し、前記第１炭化ケイ素層と前記第
２炭化ケイ素層との間に不純物を介在させない請求項７
に記載の再生炭化ケイ素被覆黒鉛材の再生法。8. After removing impurities on the surface of the first silicon carbide layer, a carbon precursor is buried in the defect, and a second layer is formed on the surface.
8. A silicon carbide layer is coated, and no impurities are interposed between the first silicon carbide layer and the second silicon carbide layer.
3. The method for regenerating a recycled silicon carbide-coated graphite material according to item 1.
理、熱処理、ハロゲン処理のいずれか１つ若しくは２つ
以上を組み合わせて除去する請求項８に記載の再生炭化
ケイ素被覆黒鉛材の再生法。9. The method of claim 8, wherein the impurities are removed by one or a combination of blasting, acid cleaning, heat treatment, and halogen treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34981399A JP2000327461A (en) | 1999-03-12 | 1999-12-09 | Regenerated graphite material coated with silicon carbide |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6705499 | 1999-03-12 | ||
| JP11-67054 | 1999-03-12 | ||
| JP34981399A JP2000327461A (en) | 1999-03-12 | 1999-12-09 | Regenerated graphite material coated with silicon carbide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000327461A true JP2000327461A (en) | 2000-11-28 |
Family
ID=26408258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34981399A Pending JP2000327461A (en) | 1999-03-12 | 1999-12-09 | Regenerated graphite material coated with silicon carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000327461A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100942353B1 (en) * | 2006-06-22 | 2010-02-12 | 가부시키가이샤 뉴플레어 테크놀로지 | Method for repairing semiconductor manufacturing apparatus, semiconductor manufacturing apparatus and method for manufacturing semiconductor |
| US20180179661A1 (en) * | 2016-12-26 | 2018-06-28 | Sumco Corporation | Method of evaluating manufacturing process of silicon material and manufacturing method of silicon material |
| CN110890309A (en) * | 2018-09-10 | 2020-03-17 | 桦榆国际有限公司 | Graphite disc repairing method |
| CN117038539A (en) * | 2023-10-10 | 2023-11-10 | 杭州海乾半导体有限公司 | Regeneration treatment method of silicon carbide epitaxial old carrier disc |
-
1999
- 1999-12-09 JP JP34981399A patent/JP2000327461A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100942353B1 (en) * | 2006-06-22 | 2010-02-12 | 가부시키가이샤 뉴플레어 테크놀로지 | Method for repairing semiconductor manufacturing apparatus, semiconductor manufacturing apparatus and method for manufacturing semiconductor |
| US20180179661A1 (en) * | 2016-12-26 | 2018-06-28 | Sumco Corporation | Method of evaluating manufacturing process of silicon material and manufacturing method of silicon material |
| JP2018107228A (en) * | 2016-12-26 | 2018-07-05 | 株式会社Sumco | Evaluating method of silicon material manufacturing process and manufacturing method of silicon material |
| US10676840B2 (en) | 2016-12-26 | 2020-06-09 | Sumco Corporation | Method of evaluating manufacturing process of silicon material and manufacturing method of silicon material |
| CN110890309A (en) * | 2018-09-10 | 2020-03-17 | 桦榆国际有限公司 | Graphite disc repairing method |
| CN110890309B (en) * | 2018-09-10 | 2023-09-08 | 桦榆国际有限公司 | Graphite disc repairing method |
| CN117038539A (en) * | 2023-10-10 | 2023-11-10 | 杭州海乾半导体有限公司 | Regeneration treatment method of silicon carbide epitaxial old carrier disc |
| CN117038539B (en) * | 2023-10-10 | 2024-01-16 | 杭州海乾半导体有限公司 | Regeneration treatment method of silicon carbide epitaxial old carrier disc |
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