JP3127011B2 - CVD reactor - Google Patents
CVD reactorInfo
- Publication number
- JP3127011B2 JP3127011B2 JP03222269A JP22226991A JP3127011B2 JP 3127011 B2 JP3127011 B2 JP 3127011B2 JP 03222269 A JP03222269 A JP 03222269A JP 22226991 A JP22226991 A JP 22226991A JP 3127011 B2 JP3127011 B2 JP 3127011B2
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- reaction
- section
- region
- reaction chamber
- 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.)
- Expired - Lifetime
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Landscapes
- Superconductors And Manufacturing Methods Therefor (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は、基板上に化学気相蒸
着法（ＣＶＤ法）を用いて被膜層を形成させる際に用い
られるＣＶＤ反応装置に係わり、更に詳しくは、超電導
マグネットコイルや電力輸送用などとして応用開発が進
められている長尺の酸化物超電導体をＣＶＤ法を用いて
製造する場合に使用されるＣＶＤ反応装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a CVD reactor used for forming a coating layer on a substrate by using a chemical vapor deposition method (CVD method). The present invention relates to a CVD reactor used for manufacturing a long oxide superconductor, which is being developed for transportation and the like by using a CVD method.
【０００２】[0002]
【従来の技術】従来、長尺の酸化物超電導体をＣＶＤ法
を用いて製造する場合、例えば図２に示されるような横
長型の反応チャンバを用いたＣＶＤ反応装置が用いられ
ている。このＣＶＤ反応装置１は、横長型の反応チャン
バ２、原料ガス供給装置３、排気ポンプ４、基板ヒータ
５、基板移送装置６を主要構成要素として備えて構成さ
れている。2. Description of the Related Art Conventionally, when a long oxide superconductor is manufactured by a CVD method, for example, a CVD reactor using a horizontally long reaction chamber as shown in FIG. 2 is used. The CVD reactor 1 includes a horizontally long reaction chamber 2, a source gas supply device 3, an exhaust pump 4, a substrate heater 5, and a substrate transfer device 6 as main components.
【０００３】上記反応チャンバ２の下方側の一端には原
料ガス供給口７が形成され、かつこの原料ガス供給口７
は、原料ガス供給管８を通じて上記原料ガス供給装置３
と接続されている。また、上記反応チャンバ２の下方側
の他端にはガス排出口９が形成され、かつこのガス排出
口９はガス排出管１０を通じて排気ポンプ４と接続され
ている。A source gas supply port 7 is formed at one end on the lower side of the reaction chamber 2.
Is connected to the source gas supply device 3 through the source gas supply pipe 8.
Is connected to A gas outlet 9 is formed at the other lower end of the reaction chamber 2, and the gas outlet 9 is connected to the exhaust pump 4 through a gas discharge pipe 10.
【０００４】また、上記反応チャンバ２内の長尺基板１
１は、基板移送装置６により図中の矢印方向に移動さ
れ、送入されるようになっている。また、さらに上記チ
ャンバ２内の下部には基板ヒータ５が設けられ、反応チ
ャンバ２内に送入される長尺基板１１を加熱できるよう
になっている。The long substrate 1 in the reaction chamber 2
1 is moved by the substrate transfer device 6 in the direction of the arrow in the figure and is sent. Further, a substrate heater 5 is provided below the chamber 2 so that the long substrate 11 fed into the reaction chamber 2 can be heated.
【０００５】上記従来のＣＶＤ反応装置１を用いて長尺
のＳＣ体を作製するには、基板移送装置６によって反応
チャンバ２内に長尺基板１１を送入し、さらに原料ガス
供給管８を介して原料ガス供給装置３からチャンバ２内
に原料ガスを導入するとともに、反応チャンバ２内を所
定の原料ガス雰囲気とする。しかる後、直ちに基板ヒー
タ６で上記チャンバ２内の長尺基板１１を加熱してこの
長尺基板１１表面にＳＣ層を蒸着させ、これによりＳＣ
体を作製することができる。In order to manufacture a long SC body using the above-mentioned conventional CVD reactor 1, a long substrate 11 is fed into the reaction chamber 2 by a substrate transfer device 6, and a raw material gas supply pipe 8 is further connected. The source gas is introduced from the source gas supply device 3 into the chamber 2 via the source gas supply system, and the inside of the reaction chamber 2 is set to a predetermined source gas atmosphere. Immediately thereafter, the long substrate 11 in the chamber 2 is immediately heated by the substrate heater 6 to deposit an SC layer on the surface of the long substrate 11, whereby the SC
The body can be made.
【０００６】[0006]
【発明が解決しようとする課題】しかしながら、上記従
来のＣＶＤ反応装置１を用いた場合、長尺基板１１は、
反応チャンバ２の入口Ａに導入されると同時に高温で急
激な加熱を受け、また、出口Ｂから搬出されると同時に
外気により急激に冷却されるため、上記反応チャンバ２
の入口及び出口において急激な温度変化を起こし、かつ
この急激な温度変化に起因する膨張あるいは収縮等の激
しいストレスが負荷される。従って、これにより基板に
「反り」や「撓み」が発生して基板の成膜面に起伏が生
ずる恐れがあるという問題があった。However, when the above-mentioned conventional CVD reactor 1 is used, the long substrate 11 is
Since it is introduced into the inlet A of the reaction chamber 2 and is rapidly heated at a high temperature at the same time as being discharged from the outlet B, it is rapidly cooled by the outside air.
Abrupt temperature changes occur at the inlet and the outlet of the device, and severe stress such as expansion or contraction caused by the rapid temperature change is applied. Therefore, there has been a problem that this may cause "warp" or "bending" of the substrate to cause undulation on the film-forming surface of the substrate.
【０００７】本発明は、上記事情に鑑みなされたもの
で、長尺基板を反応チャンバ内に導入する際、および反
応チャンバから搬出する際に、長尺基板にあるいは基板
上に蒸着されたＳＣ層に起こる温度変化を緩やかにする
ことにより、この温度変化に起因して基板あるいはＳＣ
層に発生する膨張あるいは収縮等のストレスの軽減を図
ることのでき、かつこの長尺基板上に均一かつ安定な組
成のＣＶＤ蒸着層を効率的に形成することができるＣＶ
Ｄ反応装置の提供を目的とする。SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and when introducing a long substrate into or out of the reaction chamber, an SC layer deposited on or on the long substrate. The temperature change occurring in the substrate or the SC is reduced due to this temperature change.
A CV capable of reducing stress such as expansion or contraction generated in the layer and efficiently forming a CVD deposited layer having a uniform and stable composition on the long substrate.
The purpose is to provide a D reactor.
【０００８】[0008]
【課題を解決するための手段】上記課題は、原料化合物
ガス等の原料ガスを化学反応せしめて基体表面に生成物
を堆積させるＣＶＤ反応を行う横長型の反応チャンバ
と、該反応チャンバ内に原料ガスを供給する原料ガス供
給手段と、該反応チャンバ内のガスを排気するガス排気
手段と、長尺の基体を該反応チャンバの長手方向に沿っ
て一方側に移動させる基体移動手段と、該反応チャンバ
内に配設された横長型の加熱手段とを備えたＣＶＤ反応
装置であって、前記加熱手段は、上記原料ガスを化学反
応せしめて上記基体表面に生成物を堆積させる反応温度
に該基体を加熱する反応領域と、該反応領域の基体移動
方向前方側に設けられ、上記基体が該反応領域に達する
までに該反応温度となるように該基体を漸次加熱する予
熱領域と、該反応領域の基体移動方向後方側に設けら
れ、反応温度に加熱された該基体を徐冷する徐冷領域と
を備えてなり、該反応チャンバ内に、上記反応領域両端
部に近接する遮蔽手段を設け、該反応チャンバ内を反応
部と予熱部と徐冷部とに分割し、かつ該予熱部及び該徐
冷部内に不活性ガスを送り込む不活性ガス供給手段を設
けた構成とすることにより解決される。The object of the present invention is to provide a horizontally-long reaction chamber for performing a CVD reaction in which a source gas such as a source compound gas is chemically reacted and a product is deposited on a substrate surface, and a source material is provided in the reaction chamber. Source gas supply means for supplying gas, gas exhaust means for exhausting gas in the reaction chamber, substrate moving means for moving a long substrate to one side along the longitudinal direction of the reaction chamber, A CVD reactor having a horizontal oblong heating means disposed in a chamber, wherein the heating means is set to a reaction temperature at which the source gas is chemically reacted and a product is deposited on the substrate surface. A preheating region, which is provided on the front side of the reaction region in the direction of movement of the substrate and gradually heats the substrate to reach the reaction temperature until the substrate reaches the reaction region; A slow cooling region that is provided on the rear side of the substrate moving direction and gradually cools the substrate heated to the reaction temperature, and provided in the reaction chamber, shielding means that is close to both ends of the reaction region, This problem can be solved by dividing the inside of the reaction chamber into a reaction section, a preheating section and a slow cooling section, and providing an inert gas supply means for feeding an inert gas into the preheating section and the slow cooling section. .
【０００９】[0009]
【作用】上記したように、本発明のＣＶＤ反応装置にあ
っては、加熱手段を、上記原料ガスを化学反応せしめて
上記基体表面に生成物を堆積させる反応温度に該基体を
加熱する反応領域と、該反応領域の基体移動方向前方側
に設けられ、上記基体が該反応領域に達するまでに該反
応温度となるように該基体を漸次加熱する予熱領域と、
該反応領域の基体移動方向後方側に設けられ、反応温度
に加熱された該基体を徐冷する徐冷領域とを備えてなる
構成としたので、基体を反応チャンバ内の反応領域に導
入する際、あるいは反応領域から搬出する際に、該基体
に起こる温度変化を緩やかにすることができ、これによ
り、この温度変化に起因して基体あるいはこの基体に蒸
着された薄膜に発生する膨張あるいは収縮等のストレス
が軽減される。As described above, in the CVD reaction apparatus of the present invention, the heating means is provided with a reaction region for heating the substrate to a reaction temperature at which the source gas is chemically reacted to deposit a product on the substrate surface. A preheating region that is provided on the front side of the reaction region in the substrate moving direction and that gradually heats the substrate so as to reach the reaction temperature until the substrate reaches the reaction region;
A slow cooling region provided on the rear side of the reaction region in the moving direction of the substrate and gradually cooling the substrate heated to the reaction temperature, when the substrate is introduced into the reaction region in the reaction chamber. Alternatively, the temperature change that occurs in the substrate when the substrate is unloaded from the reaction area can be moderated, whereby the expansion or contraction that occurs in the substrate or a thin film deposited on the substrate due to the temperature change can be suppressed. Stress is reduced.
【００１０】また、反応チャンバ内に、上記反応領域両
端部に近接する遮蔽手段を設け、該反応チャンバ内を反
応部と予熱部と徐冷部とに分割し、かつ該予熱部及び該
徐冷部内に不活性ガスを送り込む不活性ガス供給手段を
設けた構成としたので、反応部のみに原料ガスが供給さ
れ、予熱部及び徐冷部内には不活性ガスが供給される。
このため、良好な薄膜が得られない不十分な加熱条件で
ある予熱領域並びに徐冷領域などの領域上では成膜が行
われないので、基体上に不良薄膜が成膜されることがな
い。In the reaction chamber, shielding means are provided near both ends of the reaction area, and the inside of the reaction chamber is divided into a reaction section, a preheating section and a slow cooling section, and the preheating section and the slow cooling section are divided. Since the inert gas supply means for feeding the inert gas into the section is provided, the raw material gas is supplied only to the reaction section, and the inert gas is supplied to the preheating section and the slow cooling section.
For this reason, since a film is not formed on regions such as a preheating region and a slow cooling region, which are insufficient heating conditions under which a good thin film cannot be obtained, a defective thin film is not formed on the substrate.
【００１１】[0011]
【実施例】以下、実施例を挙げて本発明を詳細に説明す
る。図１は、本発明のＣＶＤ反応装置の一実施例を示す
ものであり、図中符号２１はＣＶＤ反応装置である。こ
のＣＶＤ反応装置２１は、横長型の反応チャンバ２２、
原料ガス供給装置２３、排気ポンプ２４、基板加熱装置
２５、基板移送装置２６を主要構成要素として備えて構
成されている。The present invention will be described below in detail with reference to examples. FIG. 1 shows an embodiment of a CVD reactor according to the present invention. In the figure, reference numeral 21 denotes a CVD reactor. The CVD reactor 21 includes a horizontally long reaction chamber 22,
The apparatus includes a source gas supply device 23, an exhaust pump 24, a substrate heating device 25, and a substrate transfer device 26 as main components.
【００１２】上記反応チャンバ２２は、その内部に設け
られた２枚の仕切部材２７，２７により、反応チャンバ
２２の長手方向中央部に位置する反応部２２ａと、この
反応部２２ａの基板移動方向前方側に位置する予熱部２
２ｂと、上記反応部２２ａの基板移動方向後方側に位置
する徐冷部２２ｃとに分けられている。また、上記反応
部２２ａの上部には、上方に向けてすぼまりかつその頂
部に原料ガス供給手段２３が接続された原料ガス拡散部
２８が形成され、予熱部２２ｂの上部および徐冷部２２
ｃの上部には、不活性ガス供給装置２９が接続されてい
る。また、上記２枚の仕切部材２７，２７下端の直下に
は、２つのガス排出口３０，３０が形成され、かつこれ
ら２つのガス排出口３０，３０はガス排出管３１を通し
て排気ポンプ２４に接続されている。The reaction chamber 22 is divided into a reaction part 22a located at the center in the longitudinal direction of the reaction chamber 22 by two partition members 27, 27 provided inside the reaction chamber 22, and a front part of the reaction part 22a in the substrate moving direction. Preheating part 2 located on the side
2b, and a slow cooling unit 22c located behind the reaction unit 22a in the substrate movement direction. A source gas diffusion section 28 is formed above the reaction section 22a and narrows upward and has a top connected to a source gas supply means 23. The upper section of the preheating section 22b and the slow cooling section 22
An inert gas supply device 29 is connected to the upper part of c. Further, two gas outlets 30, 30 are formed immediately below the lower ends of the two partition members 27, 27, and these two gas outlets 30, 30 are connected to an exhaust pump 24 through a gas exhaust pipe 31. Have been.
【００１３】上記反応チャンバ２２内の長尺基板３２
は、基板移送装置２６により図中の矢印方向に移動さ
れ、上記反応チャンバ２２内を予熱部２２ｂ→反応部２
２ａ→徐冷部２２ｃの順で通過するようになっている。
また、さらに上記チャンバ２２内の下部には予熱部２２
ｂから徐冷部２２ｃに渡る基板加熱装置２５が設けら
れ、上記反応チャンバ２２内に送入される長尺基板３２
を加熱できるようになっている。A long substrate 32 in the reaction chamber 22
Is moved by the substrate transfer device 26 in the direction of the arrow in FIG.
It passes through in the order of 2a and slow cooling section 22c.
Further, a preheating unit 22 is further provided in the lower portion of the chamber 22.
a substrate heating device 25 extending from the first substrate b to the slow cooling portion 22 c is provided, and the long substrate 32 fed into the reaction chamber 22 is provided.
Can be heated.
【００１４】上記基板加熱装置２５は、横長の熱伝導プ
レート３３と、この熱伝導プレート３３の、中央部の加
熱するヒータ３４と、上記熱伝導プレート３３の両端を
冷却する冷却器３５，３５と、上記ヒータ３４および冷
却器３５，３５を制御する温度制御装置３６とを備えて
いる。The substrate heating device 25 includes a horizontally long heat conducting plate 33, a heater 34 for heating the center of the heat conducting plate 33, and coolers 35 and 35 for cooling both ends of the heat conducting plate 33. And a temperature control device 36 for controlling the heater 34 and the coolers 35 and 35.
【００１５】また、上記構成とした基板加熱装置２５
は、反応部２２ａ内において、原料ガスを化学反応せし
めて長尺基板３２表面上に生成物を堆積させる際の反応
温度で長尺基板３２を加熱する反応領域２５ａと、予熱
部２２ｂ内において、上記長尺基板３０が反応部２２ａ
内の反応領域２５ａに到達するまでに、上記反応温度と
なるように長尺基板３２を漸次加熱する予熱領域２５ｂ
と、徐冷部２５ｃにおいて、反応温度に加熱された上記
長尺基板３２を徐冷する徐冷領域２５ｃとを備えてい
る。Further, the substrate heating device 25 having the above-described configuration is used.
In the reaction section 22a, a reaction region 25a that heats the long substrate 32 at a reaction temperature when a source gas is chemically reacted and a product is deposited on the surface of the long substrate 32, and in the preheating section 22b, The long substrate 30 is used as the reaction portion 22a.
A preheating region 25b for gradually heating the long substrate 32 so as to reach the above-mentioned reaction temperature before reaching the reaction region 25a.
And a slow cooling section 25c in which the long substrate 32 heated to the reaction temperature is gradually cooled.
【００１６】以上述べたように、本例のＣＶＤ反応装置
２１にあっては、基板加熱装置２５を、原料ガスを化学
反応せしめて長尺基板３２表面に生成物を堆積させる反
応温度に長尺基板３２を加熱する反応領域２５ａと、こ
の反応領域２５ａの基板移動方向前方側に設けられ、上
記長尺基板３２が反応領域２５ａに達するまでに上記反
応温度となるように長尺基板３２を漸次加熱する予熱領
域２５ｂと、反応領域２５ａの基板移動方向後方側に設
けられ、反応温度に加熱された長尺基板３２を徐冷する
徐冷領域２５ｃとを備えてなる構成としたので、長尺基
板３２を反応チャンバ２２内の反応領域２５ａに導入す
る際、あるいは反応領域２５ａから搬出する際に、この
長尺基板３２に起こる温度変化を緩やかにすることがで
き、これにより、この温度変化に起因して長尺基板３２
あるいはこの長尺基板３２に蒸着された薄膜に発生する
膨張あるいは収縮等のストレスが軽減される。従って、
これらストレスにより引き起こされる、例えば、基板の
成膜面への起伏の発生や、基板上に蒸着した薄膜へのク
ラックの発生を抑制することができる。また、徐冷部２
２ｃの領域にＯ2ガスを導入し、in-situ酸素処理を行う
ことにより、さらに良好な超電導テープを得ることもで
きる。As described above, in the CVD reactor 21 of the present embodiment, the substrate heating device 25 is operated at a reaction temperature at which the source gas is chemically reacted to deposit a product on the surface of the long substrate 32. A reaction region 25a for heating the substrate 32, and the long substrate 32 is provided on the front side of the reaction region 25a in the substrate moving direction so that the long substrate 32 reaches the reaction temperature until the long substrate 32 reaches the reaction region 25a. Since a preheating region 25b for heating and a slow cooling region 25c provided on the rear side of the reaction region 25a in the substrate moving direction and gradually cooling the long substrate 32 heated to the reaction temperature are provided. When the substrate 32 is introduced into the reaction region 25a in the reaction chamber 22 or when the substrate 32 is unloaded from the reaction region 25a, the temperature change occurring in the long substrate 32 can be moderated. Due to the temperature change long substrate 32
Alternatively, stress such as expansion or contraction generated in the thin film deposited on the long substrate 32 is reduced. Therefore,
For example, it is possible to suppress the occurrence of undulations on the film-forming surface of the substrate and the occurrence of cracks in the thin film deposited on the substrate, which are caused by these stresses. Also, the slow cooling unit 2
A better superconducting tape can be obtained by introducing O 2 gas into the region 2c and performing in-situ oxygen treatment.
【００１７】また、反応チャンバ２２内に、上記反応領
域２５ａ両端部に近接する仕切部材２７，２７を設け、
反応チャンバ２２内を反応部２２ａと予熱部２２ｂと徐
冷部２２ｃとに分割し、かつ予熱部２２ｂ及び徐冷部２
２ｃ内に不活性ガスを送り込む不活性ガス供給装置２９
を設けた構成としたので、反応部２２ａのみに原料ガス
が供給され、予熱部２２ｂ及び徐冷部２２ｃ内には不活
性ガスが供給される。このため、良好な薄膜が得られな
い不十分な加熱条件である予熱領域２５ｂ並びに徐冷領
域２５ｃなどの領域上では成膜が行われないので、長尺
基板３２上に不良な薄膜が成膜されるなどの不都合が防
止される。Further, in the reaction chamber 22, partition members 27, 27 close to both ends of the reaction area 25a are provided.
The inside of the reaction chamber 22 is divided into a reaction section 22a, a preheating section 22b, and a slow cooling section 22c, and the preheating section 22b and the slow cooling section 2
Inert gas supply device 29 for sending inert gas into 2c
Is provided, the source gas is supplied only to the reaction section 22a, and the inert gas is supplied to the inside of the preheating section 22b and the slow cooling section 22c. For this reason, since a film is not formed on regions such as the preheating region 25b and the slow cooling region 25c under insufficient heating conditions under which a good thin film cannot be obtained, a defective thin film is formed on the long substrate 32. Inconvenience such as being performed is prevented.
【００１８】上記本実施例のＣＶＤ反応装置２１を用
い、長尺のＳＣ体を製造するには、まず、原料ガス供給
装置２３から反応部２２ａ内に、原料ガス拡散部２７を
介してＳＣ体原料ガスを導入すると同時に、不活性ガス
供給装置２９により予熱部２２ｂおよび徐冷部２２ｃ内
にはアルゴンなどの不活性ガスを供給する。また、排気
ポンプ２４によりチャンバ２２の下方側の２つのガス排
出口３０，３０から反応部２２ａ内の反応残ガスと、予
熱部２２ｂおよび徐冷部２２ｃ内の不活性ガスを排気す
る。この時、反応部２２ａ内は、均一なＳＣ体原料ガス
雰囲気となっており、予熱部２２ｂおよび徐冷部２２ｃ
内は、不活性ガス雰囲気となっている。To manufacture a long SC body using the CVD reactor 21 of the present embodiment, first, the SC body is supplied from the raw material gas supply device 23 into the reaction section 22a through the raw material gas diffusion section 27. At the same time as the introduction of the raw material gas, an inert gas such as argon is supplied into the preheating section 22b and the slow cooling section 22c by the inert gas supply device 29. The exhaust pump 24 exhausts the residual gas in the reaction section 22a and the inert gas in the preheating section 22b and the slow cooling section 22c from the two gas outlets 30, 30 on the lower side of the chamber 22. At this time, the inside of the reaction section 22a has a uniform SC source gas atmosphere, and the preheating section 22b and the slow cooling section 22c
The inside is an inert gas atmosphere.
【００１９】次に、長尺基板３２を反応チャンバ２２内
に送入し、予熱部２２ｂ→反応部２２ａ→徐冷部２２ｃ
の順で各部内を順次通過させる。まず、はじめに不活性
ガス雰囲気の予熱部２２ｂに入った長尺基板３２は、基
板加熱装置２５の予熱領域２５ａにより、長尺基板３２
の加熱を受けている部位が、予熱部２２ｂと反応部２２
ａの境界に達するまでにＣＶＤ反応温度となるように漸
次加熱される。続いて原料ガス雰囲気の反応部２２ａに
挿入された長尺基板３２は、次の徐冷部２２ｃに達する
までに基板加熱装置２５の反応領域２５ａによってＣＶ
Ｄ反応温度で持続的に加熱され、ＳＣ体原料ガスが、加
熱された上記長尺基板３２上で反応し、この長尺基板３
２上にＳＣ層が蒸着される。さらに、このＳＣ層が蒸着
された長尺基板３２は、徐冷部２２ｃに送入されて基板
加熱装置２５の徐冷領域２５ｃによって徐冷される。Next, the long substrate 32 is fed into the reaction chamber 22, and the preheating section 22b → the reaction section 22a → the slow cooling section 22c.
, And sequentially pass through each section. First, the long substrate 32 first entering the preheating section 22b in the inert gas atmosphere is moved by the preheating region 25a of the substrate heating device 25 to the long substrate 32.
Are heated by the preheating section 22b and the reaction section 22.
Heat is gradually applied to reach the CVD reaction temperature until the boundary of a is reached. Subsequently, the long substrate 32 inserted into the reaction section 22a in the source gas atmosphere is subjected to CV by the reaction area 25a of the substrate heating device 25 before reaching the next slow cooling section 22c.
D, the SC raw material gas is continuously heated at the reaction temperature, and the SC raw material gas reacts on the heated long substrate 32.
An SC layer is deposited on 2. Further, the long substrate 32 on which the SC layer is vapor-deposited is sent to the slow cooling unit 22c and gradually cooled by the slow cooling region 25c of the substrate heating device 25.
【００２０】なお、本発明に係わるＣＶＤ反応装置を用
いてＳＣ体を製造する際において好適なＳＣ体原料とし
ては、例えばＹ−Ｂａ−Ｃｕ−Ｏ系のＳＣ体を作製する
際は、Ｙ-ビス-2,2,6,6-テトラメチル-3,5-ヘプタンジ
オナート（略称：Ｙ（ＤＰＭ）3）やＢａ-ビス-2,2,6,6
-テトラメチル-3,5-ヘプタンジオナート（略称：Ｂａ
（ＤＰＭ）2）やＣｕ-ビス-2,2,6,6-テトラメチル-3,5-
ヘプタンジオナート（略称：Ｃｕ（ＤＰＭ）2）などの
ＳＣ体原料が好適である。The SC raw material suitable for producing the SC body using the CVD reactor according to the present invention is, for example, Y-Ba-Cu-O based SC body when producing the SC body. Bis-2,2,6,6-tetramethyl-3,5-heptanedionate (abbreviation: Y (DPM) 3 ) or Ba-bis-2,2,6,6
-Tetramethyl-3,5-heptanedionate (abbreviation: Ba
(DPM) 2 ) or Cu-bis-2,2,6,6-tetramethyl-3,5-
SC raw materials such as heptane dionate (abbreviation: Cu (DPM) 2 ) are suitable.
【００２１】（実験例１）上述した実施例のＣＶＤ反応
装置２１を用いてＳＣ体を作製した。まず、原料ガス供
給装置２３から反応部２２ａ内に、Ｙ（ＤＰＭ）3、Ｂ
ａ（ＤＰＭ）2、Ｃｕ（ＤＰＭ）2より成るＳＣ体原料ガ
スを導入するとともに、不活性ガス供給装置２９により
予熱部２２ｂおよび徐冷部２２ｃ内にアルゴンガスを供
給した。同時に排気ポンプ２４により２つのガス排出口
３０，３０から所定の速度で反応部２２ａ内のガスと予
熱部２２ｂおよび徐冷部２２ｃ内のガスを排気し、反応
部２２ａ内を原料ガス雰囲気とし、予熱部２２ｂおよび
徐冷部２２ｃ内をアルゴンガス雰囲気とした。次に、上
述した操作に従って、長さ１ｍ、幅５ｍｍ、厚さ０.１
ｍｍの長尺のハステロイＣ−２７６を予熱部２２ｂ→反
応部２２ａ→徐冷部２２ｃの順で通過させ、上記長尺ハ
ステロイ上にＳＣ層が蒸着されたＳＣ体を作製した。な
お、上記ハステロイの移動速度は１ｍ／ｈとし、また、
基板加熱装置２５のヒータ３４の加熱温度を８５０℃と
し、冷却装置３５，３５の冷却温度を３０とした。(Experimental Example 1) An SC body was manufactured using the CVD reactor 21 of the above-described embodiment. First, Y (DPM) 3 , B
The SC raw material gas composed of a (DPM) 2 and Cu (DPM) 2 was introduced, and the inert gas supply device 29 supplied argon gas into the preheating unit 22b and the slow cooling unit 22c. At the same time, the gas in the reaction section 22a and the gas in the preheating section 22b and the slow cooling section 22c are exhausted from the two gas discharge ports 30, 30 at a predetermined speed by the exhaust pump 24, and the inside of the reaction section 22a is set as a raw material gas atmosphere. The inside of the preheating section 22b and the slow cooling section 22c was set to an argon gas atmosphere. Next, according to the above-described operation, the length is 1 m, the width is 5 mm, and the thickness is 0.1.
The long Hastelloy C-276 mm was passed through the preheating section 22b, the reaction section 22a, and the slow cooling section 22c in this order to produce an SC body having an SC layer deposited on the long hastelloy. The moving speed of Hastelloy is 1 m / h.
The heating temperature of the heater 34 of the substrate heating device 25 was 850 ° C., and the cooling temperatures of the cooling devices 35 and 35 were 30.
【００２２】上記操作により、長尺ハステロイ基板上
に、Ｙ−Ｂａ−Ｃｕ−Ｏ系ＳＣ層が形成された長尺ＳＣ
体を作製した。また、得られた長尺ＳＣ体のＳＣ層は、
約１０μｍの膜厚で、また、Ｘ線回折によりそのＳＣ膜
組成を調べてみたところ、その組成は均一であった。ま
た、その長尺ＳＣ体の臨界温度は、８５Ｋ以上であり、
臨界電流密度は、５０００Ａ／ｃｍ2（ａｔ７７Ｋ，０
Ｔ）であった。By the above operation, a long SC having a Y-Ba-Cu-O based SC layer formed on a long Hastelloy substrate
The body was made. In addition, the SC layer of the obtained long SC body,
When the SC film composition was examined by X-ray diffraction at a film thickness of about 10 μm, the composition was uniform. Also, the critical temperature of the long SC body is 85K or more,
The critical current density is 5000 A / cm 2 (at 77K, 0
T).
【００２３】[0023]
【発明の効果】以上述べたように、本発明のＣＶＤ反応
装置にあっては、加熱手段を、上記原料ガスを化学反応
せしめて上記基体表面に生成物を堆積させる反応温度に
該基体を加熱する反応領域と、該反応領域の基体移動方
向前方側に設けられ、上記基体が該反応領域に達するま
でに該反応温度となるように該基体を漸次加熱する予熱
領域と、該反応領域の基体移動方向後方側に設けられ、
反応温度に加熱された該基体を徐冷する徐冷領域とを備
えてなる構成としたので、基体を反応チャンバ内の反応
領域に導入する際、あるいは反応領域から搬出する際
に、該基体に起こる温度変化を緩やかにすることがで
き、これにより、この温度変化に起因して基体あるいは
この基体に蒸着された薄膜に発生する膨張あるいは収縮
等のストレスが軽減される。従って、上記ストレスによ
り引き起こされる、基体の成膜面への起伏の発生や、基
体上に蒸着した薄膜へのクラックの発生を抑制すること
ができ、例えば、本発明のＣＶＤ反応装置を用いてＳＣ
体を作製すると、臨界電流密度、臨界温度の高い良質の
ＳＣ体が得られる。As described above, in the CVD reactor of the present invention, the heating means heats the substrate to a reaction temperature at which the source gas is chemically reacted and the product is deposited on the substrate surface. A reaction region, a preheating region provided on the front side of the reaction region in the direction of movement of the substrate, and gradually heating the substrate to reach the reaction temperature until the substrate reaches the reaction region; and a substrate in the reaction region. It is provided on the rear side in the movement direction,
And a gradual cooling region for gradually cooling the substrate heated to the reaction temperature, so that when the substrate is introduced into or removed from the reaction region in the reaction chamber, The temperature change that occurs can be moderated, thereby reducing stress such as expansion or contraction that occurs in the substrate or the thin film deposited on the substrate due to the temperature change. Therefore, it is possible to suppress the occurrence of undulations on the film-forming surface of the substrate and the occurrence of cracks in the thin film deposited on the substrate, which are caused by the stress.
When the body is manufactured, a high-quality SC body having a high critical current density and a high critical temperature can be obtained.
【００２４】また、反応チャンバ内に、上記反応領域両
端部に近接する遮蔽手段を設け、該反応チャンバ内を反
応部と予熱部と徐冷部とに分割し、かつ該予熱部及び該
徐冷部内に不活性ガスを送り込む不活性ガス供給手段を
設けた構成としたので、反応部のみに原料ガスが供給さ
れ、予熱部及び徐冷部内には不活性ガスが供給される。
このため、良好な薄膜が得られない不十分な加熱条件で
ある予熱領域並びに徐冷領域などの領域上では成膜が行
われないので、基体上に不良な薄膜が成膜されるなどの
不都合が防止される。従って、例えば、本発明のＣＶＤ
反応装置を用いてＳＣ体を作製すると、臨界電流密度、
臨界温度の高い良質のＳＣ体が得られる。Further, shielding means are provided in the reaction chamber near both ends of the reaction area, and the inside of the reaction chamber is divided into a reaction section, a preheating section and a slow cooling section, and the preheating section and the slow cooling section are divided. Since the inert gas supply means for feeding the inert gas into the section is provided, the raw material gas is supplied only to the reaction section, and the inert gas is supplied to the preheating section and the slow cooling section.
For this reason, film formation is not performed on regions such as the preheating region and the slow cooling region, which are insufficient heating conditions under which a good thin film cannot be obtained, so that a disadvantageous thin film is formed on the substrate. Is prevented. Thus, for example, the CVD of the present invention
When an SC body is manufactured using a reactor, the critical current density,
A high-quality SC body having a high critical temperature can be obtained.
【図１】 本発明のＣＶＤ反応装置の一実施例を示す図
である。FIG. 1 is a view showing one embodiment of a CVD reaction apparatus of the present invention.
【図２】 従来のＣＶＤ反応装置の第１例を示す図であ
る。FIG. 2 is a diagram showing a first example of a conventional CVD reactor.
２１…ＣＶＤ反応装置、２２…反応チャンバ、２２ａ…
反応部、２２ｂ予熱部、２２ｃ…徐冷部、２３…原料ガ
ス供給装置、２４…排気ポンプ、２５…基板加熱装置、
２５ａ…反応領域、２５ｂ…予熱領域、２５ｃ…徐冷領
域、２６…基板移送装置、２７…仕切部材、２９…不活
性ガス供給装置、３２…長尺基板21 ... CVD reactor, 22 ... reaction chamber, 22a ...
Reaction section, 22b preheating section, 22c slow cooling section, 23 source gas supply device, 24 exhaust pump, 25 substrate heating device,
25a: reaction area, 25b: preheating area, 25c: slow cooling area, 26: substrate transfer device, 27: partition member, 29: inert gas supply device, 32: long substrate
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ Ｈ０１Ｌ 39/24 ＺＡＡ Ｈ０１Ｌ 39/24 ＺＡＡＢ // Ｈ０１Ｂ 12/06 ＺＡＡ Ｈ０１Ｂ 12/06 ＺＡＡ Ｈ０１Ｌ 21/31 Ｈ０１Ｌ 21/31 Ｂ (72)発明者 香川 昭 東京都江東区木場一丁目５番１号 藤倉 電線株式会社内 (72)発明者 河野 宰 東京都江東区木場一丁目５番１号 藤倉 電線株式会社内 (72)発明者 佐治 明 愛知県名古屋市緑区大高町字北関山20番 地の１ 中部電力株式会社 電力技術研 究所内 (72)発明者 黒田 昇 愛知県名古屋市緑区大高町字北関山20番 地の１ 中部電力株式会社 電力技術研 究所内 (72)発明者 吉田 弘 愛知県名古屋市緑区大高町字北関山20番 地の１ 中部電力株式会社 電力技術研 究所内 (56)参考文献 特開 昭62−227075（ＪＰ，Ａ) 特開 平１−304619（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C23C 14/00 - 14/58 C23C 16/00 - 16/56 C30B 23/00 - 25/22 H01L 21/205 H01L 21/31 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification code FI H01L 39/24 ZAA H01L 39/24 ZAAB // H01B 12/06 ZAA H01B 12/06 ZAA H01L 21/31 H01L 21/31 B ( 72) Inventor Akira Kagawa 1-5-1, Kiba, Koto-ku, Tokyo Inside Fujikura Electric Wire Co., Ltd. (72) Inventor Satoshi Kono 1-5-1, Kiba, Koto-ku, Tokyo Fujikura Electric Wire Co., Ltd. (72) Inventor Akira Saji 20-1 Kita-Sekiyama, Odaka-cho, Midori-ku, Nagoya City, Aichi Prefecture Inside the Power Technology Research Center, Chubu Electric Power Co., Inc. No. 1 Chubu Electric Power Co., Inc. Power Technology Research Institute (72) Inventor Hiroshi Yoshida 20-1 Kitakanyama, Odaka-cho, Midori-ku, Nagoya-shi, Aichi Electric Power Research Laboratory House (56) Reference Patent Sho 62-227075 (JP, A) JP flat 1-304619 (JP, A) (58 ) investigated the field (Int.Cl. 7, DB name) C23C 14/00 - 14 / 58 C23C 16/00-16/56 C30B 23/00-25/22 H01L 21/205 H01L 21/31
Claims (1)
せしめて基体表面に生成物を堆積させるＣＶＤ反応を行
う横長型の反応チャンバと、該反応チャンバ内に原料ガ
スを供給する原料ガス供給手段と、該反応チャンバ内の
ガスを排気するガス排気手段と、長尺の基体を該反応チ
ャンバの長手方向に沿って一方側に移動させる基体移動
手段と、該反応チャンバ内に配設された横長型の加熱手
段とを備えたＣＶＤ反応装置であって、前記加熱手段
は、上記原料ガスを化学反応せしめて上記基体表面に生
成物を堆積させる反応温度に該基体を加熱する反応領域
と、該反応領域の基体移動方向前方側に設けられ、上記
基体が該反応領域に達するまでに該反応温度となるよう
に該基体を漸次加熱する予熱領域と、該反応領域の基体
移動方向後方側に設けられ、反応温度に加熱された該基
体を徐冷する徐冷領域とを備えてなり、該反応チャンバ
内に、上記反応領域両端部に近接する遮蔽手段を設け、
該反応チャンバ内を反応部と予熱部と徐冷部とに分割
し、かつ該予熱部及び該徐冷部内に不活性ガスを送り込
む不活性ガス供給手段を設けたことを特徴とするＣＶＤ
反応装置。1. A horizontally elongated reaction chamber for performing a CVD reaction for chemically reacting a source gas such as a source compound gas and depositing a product on a substrate surface, and a source gas supply means for supplying the source gas into the reaction chamber Gas exhaust means for exhausting gas in the reaction chamber, substrate moving means for moving the long substrate to one side along the longitudinal direction of the reaction chamber, and a horizontally long part disposed in the reaction chamber A CVD reactor comprising: a heating section of a mold type, wherein the heating section chemically reacts the raw material gas and heats the substrate to a reaction temperature at which a product is deposited on the surface of the substrate. A preheating region that is provided on the front side of the reaction region in the substrate moving direction and gradually heats the substrate so as to reach the reaction temperature until the substrate reaches the reaction region; and a preheating region provided on the rear side of the reaction region in the substrate moving direction. And a gradual cooling region for gradually cooling the substrate heated to the reaction temperature, wherein in the reaction chamber, shielding means are provided near both ends of the reaction region,
CVD wherein the inside of the reaction chamber is divided into a reaction section, a preheating section and a slow cooling section, and inert gas supply means for feeding an inert gas into the preheating section and the slow cooling section is provided.
Reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03222269A JP3127011B2 (en) | 1991-08-07 | 1991-08-07 | CVD reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03222269A JP3127011B2 (en) | 1991-08-07 | 1991-08-07 | CVD reactor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0544043A JPH0544043A (en) | 1993-02-23 |
| JP3127011B2 true JP3127011B2 (en) | 2001-01-22 |
Family
ID=16779741
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP03222269A Expired - Lifetime JP3127011B2 (en) | 1991-08-07 | 1991-08-07 | CVD reactor |
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| Country | Link |
|---|---|
| JP (1) | JP3127011B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102958832A (en) * | 2010-06-28 | 2013-03-06 | 三星泰科威株式会社 | Graphene manufacturing apparatus and method |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040023810A1 (en) * | 2002-07-26 | 2004-02-05 | Alex Ignatiev | Superconductor material on a tape substrate |
| US20040016401A1 (en) * | 2002-07-26 | 2004-01-29 | Metal Oxide Technologies, Inc. | Method and apparatus for forming superconductor material on a tape substrate |
| JP5435473B2 (en) * | 2009-12-04 | 2014-03-05 | 古河電気工業株式会社 | Deposition method of superconducting thin film |
| JP5854853B2 (en) * | 2012-01-13 | 2016-02-09 | 古河電気工業株式会社 | CVD equipment |
-
1991
- 1991-08-07 JP JP03222269A patent/JP3127011B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102958832A (en) * | 2010-06-28 | 2013-03-06 | 三星泰科威株式会社 | Graphene manufacturing apparatus and method |
| CN102958832B (en) * | 2010-06-28 | 2016-05-25 | 韩华泰科株式会社 | Graphene manufacturing equipment and method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0544043A (en) | 1993-02-23 |
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