JPS6249350B2 - - Google Patents
Info
- Publication number
- JPS6249350B2 JPS6249350B2 JP24856786A JP24856786A JPS6249350B2 JP S6249350 B2 JPS6249350 B2 JP S6249350B2 JP 24856786 A JP24856786 A JP 24856786A JP 24856786 A JP24856786 A JP 24856786A JP S6249350 B2 JPS6249350 B2 JP S6249350B2
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- material gas
- base material
- jacket
- chemical vapor
- 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
Links
- 239000002994 raw material Substances 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000005229 chemical vapour deposition Methods 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000002093 peripheral effect Effects 0.000 claims description 5
- 239000012808 vapor phase Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 48
- 239000000758 substrate Substances 0.000 description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 239000013078 crystal Substances 0.000 description 7
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000000498 cooling water Substances 0.000 description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 229910010271 silicon carbide Inorganic materials 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000006557 surface reaction Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910003465 moissanite Inorganic materials 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Landscapes
- Chemical Vapour Deposition (AREA)
Description
【発明の詳細な説明】
本発明は例えば基材の被膜形成処理などに用い
られる化学気相蒸着装置の改良に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an improvement in a chemical vapor deposition apparatus used, for example, for forming a film on a substrate.
一般に黒鉛や金属などの表面に化学蒸着法によ
り炭化ケイ素、窒化ケイ素などの被膜を形成する
場合などには第１図の断面図に示すような化学気
相蒸着装置が使用されている。すなわち該化学気
相蒸着装置は円板形のステンレス製などのチヤン
バーベース１の上に外筒４ａ、内筒４ｂおよび天
井部４ｃからなる石英製のワークコイルカバー４
が設置され該ワークコイルカバー４内に高周波誘
導加熱用の銅製のワークコイル５が収納される。
該ワークコイル５は内筒４ｂの内側周囲を円形の
渦巻状に同一水平面上で巻かれた形状を有し両端
部５ａおよび５ｂはチヤンバーベース１に設けら
れた孔部１ａ，１ｂを通り加熱源である高周波発
振器（図示せず）に接続され加熱手段を構成して
いる。 Generally, when forming a film of silicon carbide, silicon nitride, etc. on the surface of graphite, metal, etc. by chemical vapor deposition, a chemical vapor deposition apparatus as shown in the cross-sectional view of FIG. 1 is used. That is, the chemical vapor deposition apparatus has a work coil cover 4 made of quartz, which is composed of an outer cylinder 4a, an inner cylinder 4b, and a ceiling part 4c, on a disc-shaped chamber base 1 made of stainless steel or the like.
is installed, and a copper work coil 5 for high frequency induction heating is housed within the work coil cover 4.
The work coil 5 has a circular spiral shape wound around the inner circumference of the inner cylinder 4b on the same horizontal plane, and both ends 5a and 5b pass through holes 1a and 1b provided in the chamber base 1 and are heated. The heating means is connected to a high frequency oscillator (not shown) as a source.
次に原料ガス供給部材の構造を説明する。７は
チヤンバーベース１の中央孔部１ｃと内筒４ｂ中
に挿入された下部基材ホルダーでこの上につば部
８ａを設けた上部基材ホルダー８が接続され、上
記つば部８ａ上に中央に孔を有する板状の基材９
が水平に載せられている。なお図示はしないが下
部基材ホルダー７はモータに接続され30rpm以下
に低速回転し、これにともない上部基材ホルダー
８、基材９が水平に回転する。下部基材ホルダー
７と上部基材ホルダー８の内部における軸方向の
孔部にノズルホルダー１０が挿入され、この上に
ノズル１１が隙間ばめで接合されている。ノズル
１１は上端封止部１１ａおよび水平方向放射状に
多数の噴出口１１ｂが設けられている。 Next, the structure of the raw material gas supply member will be explained. Reference numeral 7 denotes a lower base material holder inserted into the center hole 1c of the chamber base 1 and the inner tube 4b, and an upper base material holder 8 having a collar 8a is connected thereto. A plate-shaped base material 9 having holes in the
is placed horizontally. Although not shown, the lower substrate holder 7 is connected to a motor and rotates at a low speed of 30 rpm or less, and the upper substrate holder 8 and the substrate 9 rotate horizontally accordingly. A nozzle holder 10 is inserted into an axial hole inside the lower substrate holder 7 and the upper substrate holder 8, and a nozzle 11 is joined thereon by a clearance fit. The nozzle 11 is provided with an upper end sealing portion 11a and a large number of ejection ports 11b radially arranged in the horizontal direction.
なお、上記下部基材ホルダー７は電気絶縁性な
らびに断熱性をもつ石英、セラミツクなど、上部
基材ホルダー８は1000〜1600℃の耐熱性を有する
黒鉛、アルミナ、SiCなど、またノズルホルダー
１０は石英、ノズル１１は黒鉛、アルミナ、SiC
などが用いられる。 The lower substrate holder 7 is made of quartz, ceramic, etc. that have electrical insulation and heat insulation properties, the upper substrate holder 8 is made of graphite, alumina, SiC, etc. that have heat resistance of 1000 to 1600°C, and the nozzle holder 10 is made of quartz. , the nozzle 11 is made of graphite, alumina, SiC
etc. are used.
さらに反応室として２はステンレスまたは石英
製のドーム状のチヤンバーで該チヤンバー２の外
側はステンレスまたは石英製の水冷ジヤケツト３
で覆れる。チヤンバー２の下端部はチヤンバーベ
ース１の外周側に設けられたリング状の突起部１
ｄにＯリング６を介し接触しガスシールされる。
尚チヤンバー２は冷却水入口３ａから出口３ｂに
向つて流れる冷却水１５によつて冷却される。 Furthermore, the reaction chamber 2 is a dome-shaped chamber made of stainless steel or quartz, and the outside of the chamber 2 is a water-cooled jacket 3 made of stainless steel or quartz.
It can be covered with The lower end of the chamber 2 is a ring-shaped protrusion 1 provided on the outer circumferential side of the chamber base 1.
d through the O-ring 6 and is gas-sealed.
The chamber 2 is cooled by the cooling water 15 flowing from the cooling water inlet 3a toward the outlet 3b.
化学蒸着法とは高温での気相化学反応例えば揮
発性の金属のハロゲン化物や有機化合物、炭化水
素化合物などの熱分解、水素還元、置換反応など
によつて金属、黒鉛などの基材の表面に高融点金
属、炭化物、硼化物、珪化物、窒化物などの蒸着
層を形成する方法であり、上記蒸着層は加熱され
た基材表面に原料ガスが接触し核を生成し、これ
が結晶に成長することにより形成される。したが
つて上記結晶の成長速度は物質が気相から基材表
面に到達する速度すなわち気相中の物質の移動速
度と物質が結晶構造に組上げられる速度すなわち
表面反応速度により支配される。そして気相中の
物質の移動速度は気相中の物質の過飽和度および
基材表面附近におけるガスの流動状態が主な要因
となり、また一方、表面反応速度は主に反応温度
に左右される。上記中反応温度を十分高くとれば
表面反応速度は一定となるが、一方基材表面附近
におけるガスの流動状態は複雑で安定した蒸着層
の形成上問題となる。すなわち基材表面附近には
原料ガスの乱れがない層状に流れている層流境界
層のみではなく、じよう乱と呼ばれる不規則な渦
で満されている乱流境界層が形成される。この乱
流境界層においては層流境界層にくらべ基材表面
に持込まれる物質の量も多いが同時に基材表面か
ら持出される量も多くなり安定した結晶ができに
くい。さらに熱移動も活発であり急激な温度変化
を受けながら生長する被膜の結晶内部には熱応力
が残留する不具合がある。 Chemical vapor deposition is a vapor phase chemical reaction at high temperatures, such as thermal decomposition of volatile metal halides, organic compounds, hydrocarbon compounds, hydrogen reduction, substitution reactions, etc. This is a method of forming a vapor deposited layer of high melting point metal, carbide, boride, silicide, nitride, etc. on Formed by growth. Therefore, the growth rate of the crystal is controlled by the rate at which the substance reaches the surface of the substrate from the gas phase, ie, the transfer rate of the substance in the gas phase, and the rate at which the substance is assembled into a crystal structure, ie, the surface reaction rate. The transfer rate of a substance in the gas phase is mainly determined by the degree of supersaturation of the substance in the gas phase and the flow state of the gas near the surface of the substrate, while the surface reaction rate is mainly influenced by the reaction temperature. If the above-mentioned reaction temperature is set high enough, the surface reaction rate becomes constant, but on the other hand, the flow state of the gas near the surface of the substrate is complicated and poses a problem in forming a stable vapor deposited layer. That is, near the surface of the base material, not only a laminar boundary layer in which the raw material gas flows in a layered manner without turbulence, but also a turbulent boundary layer filled with irregular vortices called turbulence is formed. In this turbulent boundary layer, the amount of substances brought into the substrate surface is larger than in the laminar boundary layer, but at the same time, the amount taken out from the substrate surface is also large, making it difficult to form stable crystals. Furthermore, heat transfer is active, and there is a problem in that thermal stress remains inside the crystals of the coating, which grows while undergoing rapid temperature changes.
上記を第１図に示す従来の化学気相蒸着装置の
場合につき具体的に説明するとチヤンバー２の中
においては噴出口１１ｂからの原料ガス噴出流１
２ａおよびこれのチヤンバー２内での自然対流で
ある下降流１３、上昇流１３ａ、斜上昇流１３ｂ
を生ずるが、原料ガス１２の噴出流１２ａが上昇
流１３ａや斜上昇流１３ｂなどに衝突し、さらに
斜上昇流１３ｂの一部は基材９の側面９ｂに直接
衝突して周囲の気流はかく乱状態となる。上記の
流動状態によつて前述の乱流境界層が発生し不均
質な結晶被膜が基材表面９ａの大部分あるいは中
央部や側面９ｂに形成されることになる（尚、反
応後の排ガス１４は排気口１ｅより外部に排出さ
れる）。 To explain the above specifically in the case of the conventional chemical vapor deposition apparatus shown in FIG.
2a and its natural convection within the chamber 2, such as a downward flow 13, an upward flow 13a, and an inclined upward flow 13b.
However, the jet flow 12a of the raw material gas 12 collides with the upward flow 13a, the oblique upward flow 13b, etc., and a part of the oblique upward flow 13b directly collides with the side surface 9b of the base material 9, disturbing the surrounding airflow. state. Due to the above-mentioned flow state, the above-mentioned turbulent boundary layer is generated, and an inhomogeneous crystalline film is formed on most of the substrate surface 9a or on the center and side surfaces 9b (note that the exhaust gas 14 after the reaction is discharged to the outside from the exhaust port 1e).
本発明の目的は上記欠点のない化学気相蒸着装
置を提供することにある。 The object of the invention is to provide a chemical vapor deposition apparatus which does not have the above-mentioned disadvantages.
本発明は化学気相反応を行うための反応室と、
該反応室に原料ガスを供給する原料ガス供給部材
と、上記反応室内に被処理表面が水平となるよう
に配置される基材を加熱する加熱手段とを具備し
かつ上記原料ガス供給部材を上記基材の中央部に
設けた孔部を貫通して立設してなる化学気相蒸着
装置において、上記原料ガス供給部材を、ベンチ
ユリー形状の中空部を有し、該中空部下方の縮径
部の側面に複数個の孔部を設け上端に噴出開口部
を有する原料ガス噴出管と、該原料ガス噴出管の
外周に間隔を存して設けられ、下端に外側に湾曲
状に拡るつば部を有するジヤケツトと上方にひろ
がるラツパ管状で、かつ複数個の孔部を設けその
下縁を上記原料ガス噴出管の噴出開口部外側にま
たその上縁を上記ジヤケツトの上端内側に接続す
る接合管とから構成し、さらに基材の周囲に、該
周囲に近接し基材の上面と同じかやや高い水平部
および上方に向い湾曲する周縁部を有する皿形整
流板を具備してなる化学気相蒸着装置に関する。 The present invention includes a reaction chamber for carrying out a chemical vapor phase reaction;
The raw material gas supply member is provided with a raw material gas supply member that supplies raw material gas to the reaction chamber, and a heating means that heats a substrate disposed in the reaction chamber so that the surface to be treated is horizontal, and the raw material gas supply member is In a chemical vapor deposition apparatus that is installed vertically through a hole provided in the center of a base material, the raw material gas supply member has a ventilate-shaped hollow part, and a reduced diameter part below the hollow part. a raw material gas ejection pipe having a plurality of holes on the side surface thereof and an ejection opening at the upper end; and a collar part provided at a distance on the outer periphery of the raw material gas ejection pipe and expanding outward in a curved shape at the lower end. and a joint pipe having an upwardly extending wrapper tubular shape and having a plurality of holes, the lower edge of which is connected to the outside of the ejection opening of the raw material gas ejection pipe, and the upper edge of which is connected to the inside of the upper end of the jacket. , and further comprising a dish-shaped rectifying plate around the base material, which is close to the periphery and has a horizontal part that is the same as or slightly higher than the upper surface of the base material, and a peripheral part that curves upward. Regarding equipment.
以下図面により本発明を説明する。 The present invention will be explained below with reference to the drawings.
第２図は本発明になるチヤンバー径360mmの化
学気相蒸着装置の一実施例の概略を示す断面図で
あり、原料ガス供給部材はベンチユリー形状の原
料ガス噴出管２２、その外側に設けた内径35mmの
ジヤケツト２３及び接合管２４からなり、１８は
皿形整流板である。第３図は第２図における原料
ガス供給部材を説明する拡大断面図である。 FIG. 2 is a cross-sectional view schematically showing an embodiment of a chemical vapor deposition apparatus with a chamber diameter of 360 mm according to the present invention, in which the source gas supply member is a ventilate-shaped source gas ejection pipe 22, and an inner diameter provided on the outside thereof. It consists of a 35 mm jacket 23 and a joint tube 24, and 18 is a dish-shaped rectifying plate. FIG. 3 is an enlarged sectional view illustrating the raw material gas supply member in FIG. 2.
上記本発明の実施例に示される化学気相蒸着装
置は基材の表面積、原料ガスの供給量やチヤンバ
ー内の空間の大きさなどの設計条件に応じて特に
表面積の大きい基材の場合、該基材の表面を流れ
る原料ガスを基材の中央部までできるだけ平行に
移動する必要性のある場合に使用されるものであ
る。図において２２はノズルホルダー２１に隙間
バメ（ネジ接合でもよい）で接続された外径15mm
の原料ガス噴出管であり、原料ガス噴出管２２は
ベンチユリー形状の中空部２２ａを有し、該中空
部２２ａの縮径部２２ｂ（内径４mm）の側面に２
段８個の孔部２２ｃをまた上端に内径10mmの噴出
開口部２２ｄが設けられる。また２３は原料ガス
噴出管２２の外周に10mmの間隔を存して設けられ
下端に外側に湾曲状に拡るつば部２３ａを有し、
上端が原料ガス噴出管２２の噴出開口部２２ｄよ
りも高いジヤケツトである（高さ120mm）。また２
４は上方にひろがるラツパ管状で８個の上下方向
の孔部２４ａを有する接合管であり、接合管２４
の上縁はジヤケツト２３の上端内側にまた下縁は
原料ガス噴出管２２の噴出開口部２２ｄに接続さ
れる。なおジヤケツト２３と接合管２４とは一体
に形成しても差支えない。なおジヤケツト２３の
上端はできるだけチヤンバー２の天井中央部内壁
に接近して組立てられる。本実施例の場合は５mm
とした。またジヤケツト２３および接合管２４に
は黒鉛を使用する。 The chemical vapor deposition apparatus shown in the above embodiments of the present invention may be used depending on the design conditions such as the surface area of the substrate, the amount of raw material gas supplied, and the size of the space within the chamber. This is used when it is necessary to move the raw material gas flowing on the surface of the base material as parallel as possible to the center of the base material. In the figure, 22 is connected to the nozzle holder 21 with a clearance fit (screw connection may also be used) with an outer diameter of 15 mm.
The raw material gas jetting pipe 22 has a hollow part 22a in the shape of a ventilate, and the side surface of the reduced diameter part 22b (inner diameter 4 mm) of the hollow part 22a has two
A jet opening 22d having an inner diameter of 10 mm is provided at the upper end of the eight stages of holes 22c. Further, 23 has a flange portion 23a that is provided on the outer periphery of the raw material gas ejection pipe 22 at an interval of 10 mm and that extends outward in a curved manner at the lower end.
It is a jacket whose upper end is higher than the ejection opening 22d of the raw material gas ejection pipe 22 (height: 120 mm). Also 2
Reference numeral 4 denotes a joint pipe which is shaped like a flat tube and has eight vertical holes 24a, and the joint pipe 24
The upper edge is connected to the inside of the upper end of the jacket 23, and the lower edge is connected to the ejection opening 22d of the source gas ejection pipe 22. Note that the jacket 23 and the joint pipe 24 may be formed integrally. The upper end of the jacket 23 is assembled as close as possible to the inner wall of the ceiling center of the chamber 2. In this example, 5mm
And so. Furthermore, graphite is used for the jacket 23 and the joint tube 24.
第２図において１８は円形の基材９の周囲に取
付けられた外径345mm、内径180mmの円形の皿形整
流板であり、該皿形整流板１８は基材９の周囲に
近接する水平部１８ｂ、上方に向い湾曲する半径
50mmの周縁部１８ａからなる。なお１８ｃは皿形
整流板の下方に設けられた円筒形の脚部であり、
これによつて上記水平部１８ｂが基材９の基材表
面９ａと同一高さか、これよりやや高く配置され
る。なお上記皿形整流板１８は高さ53mmの一体品
であるが、基材９の大きさなどに応じて円周上複
数に分割してもよい。さらに材質は耐熱性のある
石英、アルミナ磁器、黒鉛等を用いる。なお第２
図の上記以外の構成は第１図の場合と同じであ
る。 In FIG. 2, reference numeral 18 denotes a circular dish-shaped rectifying plate with an outer diameter of 345 mm and an inner diameter of 180 mm attached around the circular base material 9. 18b, upwardly curved radius
It consists of a peripheral edge part 18a of 50 mm. Note that 18c is a cylindrical leg provided below the dish-shaped rectifier plate,
As a result, the horizontal portion 18b is placed at the same height as the base material surface 9a of the base material 9, or slightly higher than this. Although the dish-shaped rectifying plate 18 is a single piece with a height of 53 mm, it may be divided into a plurality of parts on the circumference depending on the size of the base material 9 and the like. Furthermore, the materials used include heat-resistant quartz, alumina porcelain, and graphite. Furthermore, the second
The configuration of the figure other than the above is the same as that of FIG. 1.
上記実施例における原料ガスの流れを説明す
る。第３図において原料ガス１２の圧力エネルギ
ーは縮径部２２ｂを通過するときに速度エネルギ
ーに変換されこの部分で減圧状態になるので側面
の複数個の孔部２２ｃから、基材表面９ａに接近
して流れるガス２５（原料ガス噴出流１２ａの水
平流）の一部は原料ガス噴出管中に吸引され、原
料ガス１２と混合しながら原料ガス噴出管２２中
を上昇し接合管２４の曲面の効果によつて水平方
向放射状に進路を変えチヤンバー２の内壁に沿つ
て下降流２５ａとして降下する。そして皿形整流
板１８の周縁部１８ａにより方向が変り水平部１
８ｂに到り水平方向に均一に整流された水平流２
５となる。一方ジヤケツト２３と原料噴出管２２
との間の空間部２３ｂは非常に高温となつている
ために活発な上昇流２５ｂも発生し、接合管２４
の孔部２４ａから吐出され前述の原料ガス噴出流
１２ａと共に水平方向放射状に流れる。なお上記
ジヤケツト２３と原料噴出管２２との空間部２３
ｂは自然対流ガスの水平流２５を基材表面９ａの
中央まで十分に吸引する作用を有する。 The flow of the raw material gas in the above embodiment will be explained. In FIG. 3, the pressure energy of the raw material gas 12 is converted into velocity energy when it passes through the diameter-reduced portion 22b, and the pressure is reduced in this portion. A part of the flowing gas 25 (horizontal flow of the raw material gas jet flow 12a) is sucked into the raw material gas jet pipe, and rises in the raw material gas jet pipe 22 while mixing with the raw material gas 12 due to the effect of the curved surface of the joint pipe 24. As a result, the flow changes its course horizontally and radially and descends along the inner wall of the chamber 2 as a downward flow 25a. Then, the direction changes due to the peripheral edge 18a of the dish-shaped rectifying plate 18, and the horizontal portion 1
Horizontal flow 2 that reaches 8b and is rectified uniformly in the horizontal direction
It becomes 5. On the other hand, the jacket 23 and the raw material spouting pipe 22
Since the space 23b between the two is at a very high temperature, an active upward flow 25b is generated, and the
The raw material gas is discharged from the hole 24a and flows radially in the horizontal direction together with the aforementioned raw material gas jet stream 12a. Note that the space 23 between the jacket 23 and the raw material ejection pipe 22
b has the function of sufficiently sucking the horizontal flow 25 of natural convection gas to the center of the base material surface 9a.
次に本発明による化学気相蒸着装置を用いた場
合と従来の装置により形成した蒸着層の特性の比
較を示す。 Next, a comparison will be made between the characteristics of deposited layers formed using the chemical vapor deposition apparatus according to the present invention and those formed using a conventional apparatus.
本発明実験例
第２図に示した装置に、中央に孔を有する直径
160mmの円板形の黒鉛基材を配置し、原料ガスと
してSiCl4及びCCl4の各12×10-3mol／分をキヤリ
アーガスH2（30／分）と共にチヤンバー内に
送り込み、反応温度1500℃（±20℃）、反応時間
60分の条件で黒鉛基材の表面にSiC層を形成し
た。Experimental Example of the Present Invention The device shown in Figure 2 has a diameter hole in the center.
A 160 mm disk-shaped graphite substrate was placed, and SiCl 4 and CCl 4 were fed into the chamber at 12 × 10 -3 mol/min each as raw material gases together with carrier gas H 2 (30/min), and the reaction temperature was set at 1500 mol/min. °C (±20 °C), reaction time
A SiC layer was formed on the surface of the graphite base material for 60 minutes.
比較実験例
一方第１図に示す従来装置に、上記本発明実験
例と同じ仕様の円板形の黒鉛基材を配置し、以下
H2ガスの流量を15／分とした以外は本発明実
験例と同一条件で上記黒鉛基材の表面にSiCの蒸
着膜を形成した。Comparative Experimental Example On the other hand, a disk-shaped graphite base material with the same specifications as the above-mentioned experimental example of the present invention was placed in the conventional apparatus shown in FIG.
A vapor deposited SiC film was formed on the surface of the graphite base material under the same conditions as in the experimental example of the present invention except that the flow rate of H 2 gas was 15/min.
上記の実験例によれば、蒸着膜の結晶粒の大き
さは従来方式では平均約20μｍであるのに対し、
本発明の場合では平均約50μｍで約２倍以上の結
晶成長が認められた。次に従来方式の場合には基
材表面の孔部の周囲と基材表面の外周部の角部に
柱状に異常に伸びた結晶が粗の状態で蒸着された
が本発明の場合には上記のような現象は認められ
なかつた。さらに上記蒸着層を形成した基材につ
いてヒートサイクルテストを行つた。すなわち上
記基材を加熱炉で400℃に加熱した後20℃の水中
に投下する試験を行つた結果、従来装置の場合に
は４回目の水中投下で蒸着層にクラツクが現れた
が、本発明の場合には13回目ではじめてクラツク
が出現した。（いずれも目視観察による）したが
つて本発明の蒸着層の耐熱衝撃性が従来装置の場
合より向上していることが判明できた。 According to the above experimental example, the average size of the crystal grains in the deposited film is about 20 μm in the conventional method, whereas
In the case of the present invention, crystal growth of about twice or more was observed with an average diameter of about 50 μm. Next, in the case of the conventional method, abnormally elongated columnar crystals were deposited in a rough state around the holes on the substrate surface and at the corners of the outer periphery of the substrate surface, but in the case of the present invention, the above No such phenomenon was observed. Furthermore, a heat cycle test was conducted on the base material on which the vapor deposited layer was formed. That is, as a result of a test in which the above-mentioned substrate was heated to 400°C in a heating furnace and then dropped into water at 20°C, cracks appeared in the vapor deposited layer after the fourth drop into water using the conventional device, but with the present invention, cracks appeared in the vapor deposition layer. In the case of , the crack appeared for the first time on the 13th time. (All results were based on visual observation) Therefore, it was found that the thermal shock resistance of the vapor deposited layer of the present invention was improved compared to that of the conventional apparatus.
このように本発明によると化学気相蒸着装置に
おける反応室内において導入する原料ガスと先に
導入され反応室内を自然対流している原料ガスと
が衝突することがないので基材の上面にこれと平
行に乱れのない原料ガスを均一に流すことができ
るため基材の全表面に均質で安定した蒸着層を形
成しうるなどその効果は極めて大である。 As described above, according to the present invention, there is no collision between the raw material gas introduced into the reaction chamber of the chemical vapor deposition apparatus and the raw material gas introduced earlier and undergoing natural convection within the reaction chamber, so that the upper surface of the substrate is coated with the raw material gas. Since the raw material gas can be uniformly flowed in parallel without turbulence, it is possible to form a homogeneous and stable vapor deposition layer on the entire surface of the base material, which is extremely effective.
第１図は従来の化学気相蒸着装置の断面図、第
２図は本発明になる化学気相蒸着装置の一実施例
の概略を示す断面図、第３図は第２図における原
料ガス供給部材を説明する拡大断面図である。
符号の説明、１……チヤンバーベース、１ａ…
…孔部、１ｂ……孔部、１ｃ……中央孔部、１ｄ
……突起部、１ｅ……排気口、２……チヤンバ
ー、３……水冷ジヤケツト、３ａ……冷却水入
口、３ｂ……冷却水出口、４……ワークコイルカ
バー、４ａ……外筒、４ｂ……内筒、４ｃ……天
井部、５……ワークコイル、５ａ，５ｂ……端
部、６……Ｏリング、７……下部基材ホルダー、
８……上部基材ホルダー、８ａ……つば部、９…
…基材、９ａ……基材表面、１０……ノズルホル
ダー、１１……ノズル、１１ａ……上端封止部、
１１ｂ……噴出口、１２……原料ガス、１２ａ…
…原料ガス噴出流、１３……下降流、１３ａ……
上昇流、１３ｂ……斜上昇流、１４……排ガス、
１５……冷却水、１８……皿形整流板、１８ａ…
…周縁部、１８ｂ……水平部、１８ｃ……脚部、
２１……ノズルホルダー、２２……原料ガス噴出
管、２２ａ……中空部、２２ｂ……縮径部、２２
ｃ……孔部、２２ｄ……噴出開口部、２３……ジ
ヤケツト、２３ａ……つば部、２３ｂ……空間
部、２４……接合管、２４ａ……孔部、２５……
水平流、２５ｂ……上昇流。
Fig. 1 is a sectional view of a conventional chemical vapor deposition apparatus, Fig. 2 is a sectional view schematically showing an embodiment of the chemical vapor deposition apparatus of the present invention, and Fig. 3 is a raw material gas supply in Fig. 2. It is an enlarged sectional view explaining a member. Explanation of symbols, 1...Chamber base, 1a...
...hole, 1b...hole, 1c...center hole, 1d
...Protrusion, 1e...Exhaust port, 2...Chamber, 3...Water cooling jacket, 3a...Cooling water inlet, 3b...Cooling water outlet, 4...Work coil cover, 4a...Outer cylinder, 4b ... Inner cylinder, 4c ... Ceiling part, 5 ... Work coil, 5a, 5b ... End part, 6 ... O ring, 7 ... Lower base material holder,
8...Upper base material holder, 8a...Brim part, 9...
... Base material, 9a ... Base material surface, 10 ... Nozzle holder, 11 ... Nozzle, 11a ... Upper end sealing part,
11b...Ejection port, 12...Source gas, 12a...
... Raw material gas jet flow, 13... Downflow, 13a...
Upflow, 13b... Oblique upflow, 14... Exhaust gas,
15...Cooling water, 18...Dish-shaped rectifying plate, 18a...
...peripheral part, 18b...horizontal part, 18c...leg part,
21... Nozzle holder, 22... Raw material gas ejection pipe, 22a... Hollow part, 22b... Diameter reduction part, 22
c... hole, 22d... jet opening, 23... jacket, 23a... collar, 23b... space, 24... joint pipe, 24a... hole, 25...
Horizontal flow, 25b...upward flow.
Claims (1)
室に原料ガスを供給する原料ガス供給部材と、上
記反応室内に被処理表面が水平となるように配置
さるる基材を加熱する加熱手段とを具備し、かつ
上記原料ガス供給部材を上記基材の中央部に設け
た孔部を貫通して立設してなる化学気相蒸着装置
において、上記原料ガス供給部材を、ベンチユリ
ー形状の中空部を有し、該中空部下方の縮径部の
側面に複数個の孔部を設け上端に噴出開口部を有
する原料ガス噴出管と、該原料ガス噴出管の外周
に間隔を存して設けられ、下端に外側に湾曲状に
拡るつば部を有するジヤケツトと上方にひろがる
ラツパ管状で、かつ複数個の孔部を設けその下縁
を上記原料ガス噴出管の噴出開口部外側にまたそ
の上縁を上記ジヤケツトの上端内側に接続する接
合管とから構成し、さらに基材の周囲に該周囲に
近接し基材の上面と同じかやや高い水平部および
上方に向い湾曲する周縁部を有する皿形整流板を
具備してなる化学気相蒸着装置。1. A reaction chamber for carrying out a chemical vapor phase reaction, a raw material gas supply member for supplying raw material gas to the reaction chamber, and heating for heating a base material placed in the reaction chamber so that the surface to be treated is horizontal. In the chemical vapor deposition apparatus, the source gas supply member is provided vertically through a hole provided in the center of the base material. A raw material gas jet pipe having a hollow part, a plurality of holes on the side surface of the reduced diameter part below the hollow part, and a jet opening at the upper end, and a space provided on the outer periphery of the raw material gas jet pipe. The jacket is provided with a jacket having a flange extending outwardly in a curved manner at the lower end, and a jacket extending upwardly in the shape of a tube and having a plurality of holes, the lower edge of which is located outside the ejection opening of the raw material gas ejection pipe. a joint pipe whose upper edge connects to the inside of the upper end of the jacket, and further has a horizontal part around the base material close to the periphery and at the same level or slightly higher than the top surface of the base material, and a peripheral edge part that curves upward. A chemical vapor deposition device equipped with a dish-shaped rectifying plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24856786A JPS62149883A (en) | 1986-10-20 | 1986-10-20 | Chemical vapor deposition device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24856786A JPS62149883A (en) | 1986-10-20 | 1986-10-20 | Chemical vapor deposition device |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15529583A Division JPS6046374A (en) | 1983-08-25 | 1983-08-25 | Chemical gaseous phase vapor deposition apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62149883A JPS62149883A (en) | 1987-07-03 |
| JPS6249350B2 true JPS6249350B2 (en) | 1987-10-19 |
Family
ID=17180062
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24856786A Granted JPS62149883A (en) | 1986-10-20 | 1986-10-20 | Chemical vapor deposition device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62149883A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19803740C2 (en) * | 1998-01-30 | 2001-05-31 | Mtu Aero Engines Gmbh | Gas phase coating method and device for gas phase coating workpieces |
-
1986
- 1986-10-20 JP JP24856786A patent/JPS62149883A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62149883A (en) | 1987-07-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4587640B2 (en) | Crystal layer deposition apparatus and crystal layer deposition method | |
| KR101167664B1 (en) | Baffled liner cover | |
| KR20120094038A (en) | Fluid bed reactor | |
| JP3414475B2 (en) | Crystal growth equipment | |
| JP2006527157A (en) | System for growing silicon carbide crystals | |
| JP2006069888A (en) | Method for manufacturing polycrystal silicon rod and manufacturing apparatus | |
| JPH06247789A (en) | Inert gas straightening and blowing device for device for pulling up single crystal | |
| TWI579419B (en) | Reactor and process for preparing granular polysilicon | |
| JPS6249350B2 (en) | ||
| JP2009071210A (en) | Susceptor and epitaxial growth system | |
| JP2018029181A (en) | Upper cone body for epitaxy chamber | |
| JPS6214222B2 (en) | ||
| US20080041309A1 (en) | Silicon Manufacturing Apparatus | |
| JPH09245957A (en) | High frequency induction heating furnace | |
| JP4354758B2 (en) | Single crystal pulling device | |
| JP4542859B2 (en) | Vapor growth equipment | |
| JP2012049316A (en) | Film deposition apparatus and film deposition method | |
| JP2011184243A (en) | Apparatus for producing chlorosilane | |
| JP6078428B2 (en) | Wafer support and chemical vapor deposition apparatus using the wafer support | |
| JP6413925B2 (en) | Silicon carbide single crystal manufacturing equipment | |
| CN220012799U (en) | Temperature control part and CVD reaction device | |
| JPS6254081A (en) | Vapor growth device | |
| WO2024045822A1 (en) | Temperature control component and cvd reaction device | |
| JP4515227B2 (en) | Vapor growth equipment | |
| JPH06232054A (en) | Manufacture of susceptor |