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JP4832046B2 - Continuous thermal CVD equipment - Google Patents
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JP4832046B2 - Continuous thermal CVD equipment - Google Patents

Continuous thermal CVD equipment Download PDF

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JP4832046B2
JP4832046B2 JP2005285733A JP2005285733A JP4832046B2 JP 4832046 B2 JP4832046 B2 JP 4832046B2 JP 2005285733 A JP2005285733 A JP 2005285733A JP 2005285733 A JP2005285733 A JP 2005285733A JP 4832046 B2 JP4832046 B2 JP 4832046B2
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gas
substrate
conveyor
cvd
heating zone
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JP2007092152A (en
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百世 澤井
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Kanadevia Corp
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Hitachi Zosen Corp
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Description

本発明は、膜やカーボンナノチューブの製造などに使用されるベルトコンベヤを主体する連続熱CVD装置に関するものである。   The present invention relates to a continuous thermal CVD apparatus mainly comprising a belt conveyor used for production of a film or a carbon nanotube.

化学気相蒸着法(以下CVD法という)による膜の形成方法は、不活性ガス雰囲気で反応管内に基板を設置し、反応管内に原料ガスを送り込み、基板上に設けられた触媒微粒子を核として基板表面に膜やカーボンナノチューブを形成する方法である。CVD法は、熱を利用する熱CVD法、プラズマを利用するプラズマCVD法、光エネルギーを利用する光CVD法に分けられる。また、CVD装置は、膜を減圧状態で形成する減圧CVD装置と、大気圧で行う常圧CVD装置に分けられる。   A film formation method by chemical vapor deposition (hereinafter referred to as CVD method) is a method in which a substrate is placed in a reaction tube in an inert gas atmosphere, a raw material gas is sent into the reaction tube, and catalyst fine particles provided on the substrate are used as nuclei. In this method, a film or a carbon nanotube is formed on the substrate surface. The CVD method is classified into a thermal CVD method using heat, a plasma CVD method using plasma, and a photo CVD method using light energy. Further, the CVD apparatus is classified into a low pressure CVD apparatus that forms a film in a reduced pressure state and an atmospheric pressure CVD apparatus that performs at atmospheric pressure.

熱CVD装置としては、反応器に1枚または複数枚の基板を一度に供給して膜を形成するバッチ式のものが一般的である。この装置では、一度反応を行うと、その都度、反応器内の基板やガスの置換が必要であるため、操作時間が長くかかる上に、多量のキャリアガスおよび原料ガスを必要とし、一度に大量の基板を供給することは困難であった。このため、基板をベルトコンベア等の搬送手段により連続的に反応器内に供給し、膜を生成させる連続式のCVD装置が開発されている(特許文献1参照)。
特開2000−77340号公報
As a thermal CVD apparatus, a batch type apparatus in which one or a plurality of substrates is supplied to a reactor at a time to form a film is generally used. In this apparatus, once a reaction is performed, it is necessary to replace the substrate and gas in the reactor each time. Therefore, the operation time is long, and a large amount of carrier gas and source gas are required. It was difficult to supply the substrate. For this reason, a continuous CVD apparatus has been developed in which a substrate is continuously supplied into a reactor by a conveying means such as a belt conveyor to generate a film (see Patent Document 1).
JP 2000-77340 A

しかしながら、反応器内に基板を連続的に供給して常圧で膜を生成させる常圧CVD装置においては、反応器内雰囲気とその外気との間のシールが不充分であると、反応器内に不純物ガス成分やパーティクルが混入し、基板表面における膜の生成が不均一になり、パーティクルが基板に付着する等のため、製品の歩留まりが低いという問題があった。また、従来のCVD装置では、バッチ式、連続式を問わず、反応器内において原料ガスの供給または加熱の際に基板近傍での基板・ガスの温度分布およびガス流れの制御が困難で、温度分布およびガス流れにむらができ易く、これが基板上に形成される膜の均一性低下の要因となっていた。   However, in an atmospheric pressure CVD apparatus in which a substrate is continuously supplied into the reactor to form a film at atmospheric pressure, if the seal between the atmosphere in the reactor and its outside air is insufficient, Impurity gas components and particles are mixed into the substrate, resulting in non-uniform film formation on the substrate surface, and particles adhering to the substrate, resulting in a low product yield. Also, with conventional CVD devices, it is difficult to control the temperature distribution and gas flow of the substrate and gas in the vicinity of the substrate when supplying or heating the source gas in the reactor, regardless of whether it is a batch type or a continuous type. The distribution and the gas flow are likely to be uneven, which has been a factor in reducing the uniformity of the film formed on the substrate.

本発明は、上記諸問題に鑑み、反応器内へ不純物ガス成分やパーティクルが混入する恐れがなく、基板近傍での基板・ガスの温度分布およびガス流れの制御がし易くて均―性の高い膜の形成が可能である連続熱CVD装置を提供することを課題とする。   In view of the above problems, the present invention has high uniformity because it is easy to control the temperature distribution and gas flow of the substrate and gas in the vicinity of the substrate without the possibility of impurity gas components and particles entering the reactor. It is an object of the present invention to provide a continuous thermal CVD apparatus capable of forming a film.

本発明は、水平に配されたループ状のベルトコンベヤと、コンベヤの一端部上に供給された基板と、コンベヤの一側の長さ中央部から他端円弧部に亘って設けられた基板予熱ゾーンと、コンベヤの他側にその他端部から長さ中央部に亘って設けられたCVD加熱ゾーンと、コンベヤの他端他側に設けられたキャリアガス流入口と、該キャリアガス流入口内の上部にCVD加熱ゾーン向きに設けられた原料ガス流入口とを備え、該原料ガス流入口の延長部は、ベルトコンベヤの他端円弧部の他側部の上まで至り、該延長部は基板より幅広なノズルを有する、連続CVD装置を提供する。
The present invention relates to a loop belt conveyor arranged horizontally, a substrate supplied on one end of the conveyor, and a substrate preheating provided from the central portion of the length of one side of the conveyor to the arc portion of the other end. A zone, a CVD heating zone provided from the other end to the center of the length on the other side of the conveyor, a carrier gas inlet provided on the other end of the conveyor, and an upper portion in the carrier gas inlet Bei example a feed gas inlet provided in the CVD heating zone facing the extension portion of the raw material gas inlet is led to the top of the other side of the other end arc part of the belt conveyor, the extension portion from the substrate A continuous CVD apparatus having a wide nozzle is provided.

本発明による連続CVD装置は、好ましくは、原料ガスの未反応分とキャリアガスとのガス混合物を排出する排気路と、排気路に隣接して設けられたシールガス給気路とを備える。   The continuous CVD apparatus according to the present invention preferably includes an exhaust path for discharging a gas mixture of unreacted raw material gas and carrier gas, and a seal gas supply path provided adjacent to the exhaust path.

なお、本明細書においては、図1に示される連続CVD装置の右端を一端とし、左端を他端とし、上側を一側とし、下側を他側とする。   In this specification, the right end of the continuous CVD apparatus shown in FIG. 1 is one end, the left end is the other end, the upper side is one side, and the lower side is the other side.

本発明による連続CVD装置は、コンベヤの一側の長さ中央部から他端円弧部に亘って設けられた基板予熱ゾーンと、コンベヤの他側にその他端部から長さ中央部に亘って設けられたCVD加熱ゾーンとを備え、これらのゾーンにおいてコンベヤの必要な部分だけを加熱するので、コンベヤ全体を加熱する装置に比べ省エネルギーが達成でき、製品のコストを削減することができる。   The continuous CVD apparatus according to the present invention is provided with a substrate preheating zone provided from the central length of one side of the conveyor to the arc of the other end, and provided from the other end to the central length of the other side of the conveyor. Since only the necessary portions of the conveyor are heated in these zones, energy saving can be achieved as compared with an apparatus for heating the entire conveyor, and the cost of the product can be reduced.

また、この装置はコンベヤの他端他側にキャリアガスの流入口を備えるので、同ガスの一部を予熱ゾーンへ流入させることによって、予熱ゾーンで予熱されたガスが同ゾーンからCVD加熱ゾーンへ流入するのを防ぐことができ、これにより予熱ガスに含まれる不純物ガス成分やパーティクルがCVD加熱ゾーンに混入するのを確実に防ぐことができ、製品の歩留まりを向上することができる。   In addition, since this apparatus is provided with a carrier gas inlet on the other end of the conveyor, by flowing a part of the gas into the preheating zone, the gas preheated in the preheating zone is transferred from the zone to the CVD heating zone. It is possible to prevent the inflow of impurities, thereby reliably preventing impurity gas components and particles contained in the preheating gas from entering the CVD heating zone, and improving the yield of products.

加えて、この装置によれば、基板が基板予熱ゾーンおよびCVD加熱ゾーンを移動させられることで、生成面積の制限がなくなり、均一で且つ大面積の膜を生成することができる。   In addition, according to this apparatus, since the substrate is moved between the substrate preheating zone and the CVD heating zone, the generation area is not limited, and a uniform and large-area film can be generated.

さらに、排気路に隣接してシールガス給気路を設けることにより、外気がCVD加熱ゾーンへ流入するのを防ぐことができ、外気に含まれる不純物ガス成分やパーティクルがCVD加熱ゾーンに混入するのを確実に防ぐことができる。   Furthermore, by providing a seal gas supply passage adjacent to the exhaust passage, it is possible to prevent the outside air from flowing into the CVD heating zone, and impurity gas components and particles contained in the outside air are mixed into the CVD heating zone. Can be surely prevented.

つぎに、本発明を具体的に説明するために、本発明の実施形態を示す。   Next, in order to describe the present invention specifically, an embodiment of the present invention is shown.

図1、図2において、両側ストレート部と両端円弧部からなるループ状のベルトコンベヤ(1) が水平に配されている。ベルトコンベヤ(1) の一端一側上に、触媒(図示省略)を担持したシリコン製の基板(4) が連続的に供給される。この基板搬入部の回転方向前方にはケーシング(5) の頂壁に立上がり状に排気路(13)が設けられ、これによりキャリアガス等を含むガス混合物が装置外へ排出される。ベルトコンベヤ(1) は、その一端寄りの部分を除いて、水平断面略U字状のケーシング(5) に収められている。ベルトコンベヤ(1) の一側の長さ中央部から他端円弧部に亘って予熱ゾーン(9) が設けられている。   In FIG. 1 and FIG. 2, a loop belt conveyor (1) composed of straight sections on both sides and circular arc sections on both ends is horizontally arranged. On one end of the belt conveyor (1), a silicon substrate (4) carrying a catalyst (not shown) is continuously supplied. An exhaust passage (13) is provided on the top wall of the casing (5) so as to rise in front of the substrate carrying-in portion in the rotational direction, whereby a gas mixture containing a carrier gas and the like is discharged out of the apparatus. The belt conveyor (1) is housed in a casing (5) having a substantially U-shaped horizontal section except for a portion near one end thereof. A preheating zone (9) is provided from the length central portion on one side of the belt conveyor (1) to the arc portion on the other end.

ベルトコンベヤ(1) の他側には、他端部から長さ中央部に亘ってCVD加熱ゾーン(11)が設けられている。予熱ゾーン(9) とその回転方向前方のCVD加熱ゾーン(11)は、図中で一点鎖線(a) で示すように連続しており、加熱手段(図示省略)で所要温度に加熱される。   On the other side of the belt conveyor (1), a CVD heating zone (11) is provided from the other end to the center of the length. The preheating zone (9) and the CVD heating zone (11) in front of the rotation direction are continuous as shown by a one-dot chain line (a) in the figure, and are heated to a required temperature by heating means (not shown).

ベルトコンベヤ(1) を収めたケーシング(5) の他端他側にはその垂直端壁(12)にキャリアガスの流入口(2) が水平に設けられ、同流入口(2) 内の上部に原料ガス流入口(3) がCVD加熱ゾーン(11)向きに水平に設けられ、その延長部(6) はベルトコンベヤ(1) の他端円弧部の他側部の上まで至る。原料ガス流入口(3) の延長部(6) は、基板(4) より幅広な偏平ノズル(6a)を有する(幅100mm×高さ5mm)。偏平ノズル(6a)の下壁先端部(6b)は前方下向きに傾いた傾斜壁となされている。このような構成により、原料ガスとキャリアガスの混合ガスが偏平ノズル(6a)から基板(4) 上に均等に供給され、偏平ノズル(6a)と基板(4) の間にキャリアガスが流される。キャリアガスは、原料ガスをケーシング(5) の他端他側からCVD加熱ゾーン(11)へ導入してケーシング(5) の他側部の内部を通過させる。キャリアガスはまた、基板予熱ゾーン(9) からCVD加熱ゾーン(11)へのガス流入を防ぐ働きをし、さらに原料ガスとキャリアガスの混合ガスが逆流して漏れ出るのを完全に防ぐシールガスとしても働く。原料ガスとキャリアガスの混合ガスを偏平ノズル(6a)から基板(4) 上に一様に供給することにより、基板(4) 表面に形成される膜(7) の厚さを均一化することができる。また、シールガスとしてのキャリアガス、および、原料ガスとキャリアガスの混合ガスの供給量および/または濃度を適時制御することにより、所望の均一な厚さの膜(7) が形成できる。   On the other end of the casing (5) containing the belt conveyor (1), a carrier gas inlet (2) is provided horizontally on the vertical end wall (12), and the upper part in the inlet (2) The material gas inlet (3) is horizontally provided in the direction of the CVD heating zone (11), and its extension (6) extends to the other side of the other end arc portion of the belt conveyor (1). The extension part (6) of the raw material gas inlet (3) has a flat nozzle (6a) wider than the substrate (4) (width 100 mm × height 5 mm). The lower wall tip (6b) of the flat nozzle (6a) is an inclined wall inclined forward and downward. With such a configuration, the mixed gas of the source gas and the carrier gas is evenly supplied onto the substrate (4) from the flat nozzle (6a), and the carrier gas flows between the flat nozzle (6a) and the substrate (4). . The carrier gas introduces the source gas from the other side of the other end of the casing (5) into the CVD heating zone (11) and passes the inside of the other side of the casing (5). The carrier gas also serves to prevent gas flow from the substrate preheating zone (9) to the CVD heating zone (11), and further prevents the mixed gas of the source gas and carrier gas from flowing backward and completely leaking out. Work as well. Uniform thickness of the film (7) formed on the surface of the substrate (4) by uniformly supplying a mixed gas of source gas and carrier gas from the flat nozzle (6a) onto the substrate (4) Can do. Moreover, a film (7) having a desired uniform thickness can be formed by appropriately controlling the supply amount and / or concentration of the carrier gas as the seal gas and the mixed gas of the source gas and the carrier gas.

CVD加熱ゾーン(11)より回転方向前方にはケーシング(5) の頂壁に立上がり状に排気路(8) が設けられ、これにより原料ガスの未反応分とキャリアガスとのガス混合物が装置外へ排出される。排気路(8) のさらに回転方向前方にはこれに隣接してシールガスの給気路(10)が設けられている。   An exhaust passage (8) is provided on the top wall of the casing (5) so as to rise in front of the CVD heating zone (11) in the direction of rotation, so that a gas mixture of unreacted raw material gas and carrier gas is removed from the outside of the apparatus. Is discharged. A seal gas supply passage (10) is provided adjacent to the exhaust passage (8) in front of the rotation direction.

上記構成の膜の連続製造装置において、複数の基板(4) がベルトコンベヤ(1) の一端一側からコンベヤのベルト上に連続的に供給される。次いで基板(4) は予熱ゾーン(9) へ送られ、ここで予熱され、ベルトコンベヤ(1) の他端円弧部を通過してCVD加熱ゾーン(11)に入る。予熱ゾーン(9) には、流入口(2) からキャリアガス(ヘリウムガス、アルゴンガスなどの不活性ガス)の一部が送り込まれる。これによって、予熱ゾーン(9) で予熱されたガスが同ゾーン(9) からCVD加熱ゾーン(11)へ流入するのを防ぐことができ、予熱ガスに含まれる不純物ガス成分やパーティクルがCVD加熱ゾーンに混入するのを確実に防ぐことができる。   In the continuous film production apparatus having the above-described configuration, a plurality of substrates (4) are continuously supplied from one end of the belt conveyor (1) onto the conveyor belt. The substrate (4) is then sent to a preheating zone (9) where it is preheated and passes through the other end arc of the belt conveyor (1) to enter the CVD heating zone (11). A part of the carrier gas (inert gas such as helium gas or argon gas) is fed into the preheating zone (9) from the inlet (2). This prevents the gas preheated in the preheating zone (9) from flowing into the CVD heating zone (11) from the zone (9), and the impurity gas components and particles contained in the preheating gas are prevented from flowing into the CVD heating zone. Can be surely prevented.

CVD加熱ゾーン(11)には、原料ガス流入口(3) から原料ガス通路(6) を経て来た膜形成用の原料ガスと、キャリアガス流入口(2) からのキャリアガスの残部とのガス混合物が供給される。これによって、基板(4) 表面に膜(7) が形成される。膜(7) 付き基板(4)
は、次いでケーシング(5) を出てベルトコンベヤ(1) から装置外へ搬出される。基板搬入部の回転方向前方に隣接してケーシング(5) の一側一端にも、シールガス給気路(10)と同じ構造のシールガス給気路(14)が設けられている。
In the CVD heating zone (11), the raw material gas for film formation from the raw material gas inlet (3) through the raw material gas passage (6) and the remainder of the carrier gas from the carrier gas inlet (2) A gas mixture is supplied. As a result, a film (7) is formed on the surface of the substrate (4). Substrate with membrane (7) (4)
Next, it leaves the casing (5) and is carried out of the apparatus from the belt conveyor (1). A seal gas supply passage (14) having the same structure as the seal gas supply passage (10) is provided at one end of the casing (5) adjacent to the front of the substrate carrying-in portion in the rotation direction.

原料ガスの未反応分とキャリアガスとのガス混合物は、排気路(8) を経て装置外へ排出される。シールガスが給気路(10)(14)を経てケーシング(5) 内に吹き込まれる。これによって、外気がケーシング(5) の回転方向前方および基板搬入部からCVD加熱ゾーン(11)へ流入するのを防ぐことができ、外気に含まれる不純物ガス成分やパーティクルがCVD加熱ゾーンに混入するのを確実に防ぐことができる。   The gas mixture of the unreacted material gas and the carrier gas is discharged out of the apparatus through the exhaust path (8). Seal gas is blown into the casing (5) through the air supply passages (10), (14). This prevents outside air from flowing into the CVD heating zone (11) from the front of the casing (5) in the rotation direction and from the substrate carry-in portion, and impurity gas components and particles contained in the outside air are mixed into the CVD heating zone. Can be surely prevented.

膜連続製造装置を示す平面図である。It is a top view which shows a film | membrane continuous manufacturing apparatus. 膜連続製造装置を示す垂直縦断面図である。It is a vertical longitudinal cross-sectional view which shows a film | membrane continuous manufacturing apparatus.

符号の説明Explanation of symbols

(1) :ループ状のベルトコンベヤ
(2) :キャリアガス流入口
(3) :原料ガス流入口
(4) :基板
(5) :ケーシング
(6) :延長部
(6a):偏平ノズル
(8) (13):排気路
(9) :予熱ゾーン
(10)(14):シールガス給気路
(11):CVD加熱ゾーン
(12):垂直壁
(1): Loop belt conveyor
(2): Carrier gas inlet
(3): Raw material gas inlet
(4): Board
(5): Casing
(6): Extension
(6a): Flat nozzle
(8) (13): Exhaust passage
(9): Preheating zone
(10) (14): Seal gas supply passage
(11): CVD heating zone
(12): Vertical wall

Claims (2)

水平に配されたループ状のベルトコンベヤと、コンベヤの一端部上に供給された基板と、コンベヤの一側の長さ中央部から他端円弧部に亘って設けられた基板予熱ゾーンと、コンベヤの他側にその他端部から長さ中央部に亘って設けられたCVD加熱ゾーンと、コンベヤの他端他側に設けられたキャリアガス流入口と、該キャリアガス流入口内の上部にCVD加熱ゾーン向きに設けられた原料ガス流入口とを備え、該原料ガス流入口の延長部は、ベルトコンベヤの他端円弧部の他側部の上まで至り、該延長部は基板より幅広なノズルを有する、連続CVD装置。 Horizontally arranged loop belt conveyor, substrate supplied on one end of the conveyor, substrate preheating zone provided from the center of the length of one side of the conveyor to the arc of the other end, the conveyor A CVD heating zone provided on the other side from the other end to the center of the length, a carrier gas inlet provided on the other side of the other end of the conveyor, and a CVD heating zone on the upper side in the carrier gas inlet e Bei a feed gas inlet provided in the orientation, the extension of the raw material gas inlet is led to the top of the other side of the other end arc part of the belt conveyor, said extension portion is a wider nozzle from the substrate A continuous CVD apparatus. 原料ガスの未反応分とキャリアガスとのガス混合物を排出する排気路と、排気路に隣接して設けられたシールガス給気路とを備えた請求項1記載の連続CVD装置。   The continuous CVD apparatus according to claim 1, further comprising: an exhaust path for discharging a gas mixture of unreacted raw material gas and carrier gas; and a seal gas supply path provided adjacent to the exhaust path.
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