JPH0535223B2 - - Google Patents

Info

Publication number
JPH0535223B2
JPH0535223B2 JP61060730A JP6073086A JPH0535223B2 JP H0535223 B2 JPH0535223 B2 JP H0535223B2 JP 61060730 A JP61060730 A JP 61060730A JP 6073086 A JP6073086 A JP 6073086A JP H0535223 B2 JPH0535223 B2 JP H0535223B2
Authority
JP
Japan
Prior art keywords
reaction
vapor deposition
deposited
reaction chamber
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 - Lifetime
Application number
JP61060730A
Other languages
Japanese (ja)
Other versions
JPS62218574A (en
Inventor
Shigeo Mizoguchi
Yasunobu Yoshinaga
Kazuo Abe
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHINKU ZAIRYO KK
Original Assignee
SHINKU ZAIRYO KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by SHINKU ZAIRYO KK filed Critical SHINKU ZAIRYO KK
Priority to JP6073086A priority Critical patent/JPS62218574A/en
Publication of JPS62218574A publication Critical patent/JPS62218574A/en
Publication of JPH0535223B2 publication Critical patent/JPH0535223B2/ja
Granted legal-status Critical Current

Links

Description

【発明の詳細な説明】 [産業上の利用分野] 本発明は、化学反応により被蒸着物上に高純度
の金属化合物膜または単体の金属膜を形成する化
学蒸着装置に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a chemical vapor deposition apparatus that forms a highly pure metal compound film or a single metal film on an object to be deposited by chemical reaction.

[従来の技術] 従来、化学蒸着を行なう場合、原料となる有機
金属や金属ハロゲン化物を、反応を行なう反応室
とは別個に容器等に収納して設置し、これらの有
機金属や金属ハロゲン化物を加熱等によりガス化
して、流量計やパイプを介して反応室内の被蒸着
物上へ流し込み、反応室内で反応を完成させ被蒸
着物上に金属化合物膜または単体の金属膜を積層
する方法が一般に用いられてきた。
[Prior art] Conventionally, when performing chemical vapor deposition, organic metals and metal halides as raw materials are stored and installed in a container separate from the reaction chamber in which the reaction takes place, and these organic metals and metal halides are There is a method in which the gas is gasified by heating, etc., and poured onto the object to be deposited in the reaction chamber through a flowmeter or pipe, the reaction is completed in the reaction chamber, and a metal compound film or a single metal film is laminated on the object to be evaporated. It has been commonly used.

このような方法を実施するための種々の装置が
提案され、実用に供されている。
Various devices for carrying out such methods have been proposed and put into practical use.

[発明が解決しようとする課題] ところで、このような従来の方法では、原料か
らの腐蝕性のあるガスや毒性のあるガス等が流量
計やパイプを通る間に不純物が混入したり、ガス
成分の化学組成が変化し、このため、反応室内に
挿置された被蒸着物上の蒸着膜中に不純物が混入
したり、あるいは温度の低下等によつてパイプ内
部においてガスが固化したり液化したりしてパイ
プを詰らせるという欠点がある。
[Problems to be Solved by the Invention] However, in such conventional methods, impurities may be mixed in while corrosive gases or toxic gases from raw materials pass through flowmeters or pipes, or gas components may be mixed in. The chemical composition of the gas may change, and as a result, impurities may be mixed into the vapor deposited film on the object placed in the reaction chamber, or the gas may solidify or liquefy inside the pipe due to a drop in temperature, etc. The disadvantage is that it can clog the pipes.

これらの欠点を解消するため、気化した原料の
導入パイプに高価なテフロンを内張りしたり、高
純度に精製加工したパイプを使用したり、また温
度の低下を防止するためパイプの周辺に加熱手段
を設ける等の対策が取られてきたが、このような
手段には材料費が高くなりコスト負担が大きく、
しかも品質管理上の問題等多くの問題点を含んで
いる。
In order to eliminate these drawbacks, the introduction pipe for the vaporized raw material is lined with expensive Teflon, the pipe is purified to a high degree of purity, and heating means are installed around the pipe to prevent the temperature from dropping. Countermeasures have been taken, such as installing a
Moreover, it includes many problems such as quality control problems.

そこで、本発明の目的は、パイプ等からの不純
物や気体分子の形態変化による不純物等を含むこ
となしに気化した原料を反応室内に挿置された被
蒸着物の表面上に導き、不純物を実質的に含まな
い高純度の金属化合物薄膜または単体の金属薄膜
を所望の組成で形成することのできる化学蒸着装
置を提供することにある。
Therefore, an object of the present invention is to introduce a vaporized raw material from a pipe etc. without containing impurities or impurities due to a change in the form of gas molecules onto the surface of an object to be deposited placed in a reaction chamber, thereby substantially removing impurities. It is an object of the present invention to provide a chemical vapor deposition apparatus capable of forming a high-purity metal compound thin film or a single metal thin film with a desired composition.

[課題を解決するための手段] 上記の目的を達成するために、本発明による化
学蒸着装置は、内部に被蒸着物を支持する支持部
材を備え、プラズマ放電により反応を行うように
した反応室に直結して、複数の蒸発室を設け、各
蒸発室には、有機金属または金属ハロゲン化物材
料を収容する、それら材料を構成している金属か
ら成る容器と、上記容器を加熱して上記容器内の
化合物を気化させる加熱手段とを設け、また各蒸
発室内の容器から気化した上記材料の反応室内へ
の流量を制御するキヤリアガス供給系を各蒸発室
に対して別個に設け、反応室内の上記被蒸着物の
表面上に所望の組成をもつ金属化合物薄膜または
単体の金属薄膜を形成できるように構成したこと
を特徴としている。
[Means for Solving the Problems] In order to achieve the above object, a chemical vapor deposition apparatus according to the present invention includes a reaction chamber which is provided with a support member for supporting a material to be deposited therein and is configured to perform a reaction by plasma discharge. A plurality of evaporation chambers are provided directly connected to the evaporation chamber, each evaporation chamber containing a container made of the metal constituting the organometallic or metal halide material, and a container made of the metal constituting the organometallic or metal halide material; A carrier gas supply system is provided separately for each evaporation chamber to control the flow rate of the material vaporized from the container in each evaporation chamber into the reaction chamber. It is characterized by being configured so that a metal compound thin film or a single metal thin film having a desired composition can be formed on the surface of an object to be deposited.

被蒸着物を支持する支持部材は好ましくは反応
動作中回転するようにされた回転体から成ること
ができる。
The support member for supporting the material to be deposited can preferably consist of a rotating body that is adapted to rotate during the reaction operation.

また、反応室は反応により副生した排ガスをキ
ヤリアガスと共に系外へ排出する排気口を備える
ことができる。
Further, the reaction chamber can be provided with an exhaust port for discharging exhaust gas by-produced by the reaction out of the system together with the carrier gas.

[作用] 本発明による化学蒸着装置では、ガス化した原
料の有機金属またはハロゲン化物金属はパイプ等
の中を通過することなしに直接反応室内の被蒸着
物の表面に導入することができ、従つて不純物や
気体分子の形態変化による不純物等を含むことな
しにプラズマ反応が行なわれ、被蒸着物の表面に
蒸着される。これによつて、薄膜中への不純物の
混入を防止することができる。またガス化した有
機金属またはハロゲン化物金属を直接反応室内の
被蒸着物の表面に導入することができるので、気
化した分子の経時変が伴わない。このため気化し
た分子が液化または固化することなく操作が容易
でかつ品質の良い蒸着物を得ることができる。
[Function] In the chemical vapor deposition apparatus according to the present invention, the organic metal or halide metal as the gasified raw material can be introduced directly onto the surface of the object to be deposited in the reaction chamber without passing through a pipe or the like. As a result, a plasma reaction is performed without including impurities or impurities caused by changes in the form of gas molecules, and the vapor is deposited on the surface of the object to be vaporized. This can prevent impurities from entering the thin film. Furthermore, since the gasified organic metal or metal halide can be directly introduced onto the surface of the object to be deposited in the reaction chamber, the vaporized molecules do not change over time. Therefore, the vaporized molecules do not liquefy or solidify, making it possible to easily operate and obtain a vapor deposit of good quality.

さらに、本発明では、各蒸発室に別個に、気化
した上記材料の反応室内への流量を制御するキヤ
リアガス供給系を設けているので、各蒸発室に導
入するキヤリアガスの流量を調整するだけで蒸着
物の表面に蒸着させる化合物の組成を調整するこ
とができるようになる。
Furthermore, in the present invention, since each evaporation chamber is provided with a separate carrier gas supply system that controls the flow rate of the vaporized material into the reaction chamber, vapor deposition can be performed simply by adjusting the flow rate of the carrier gas introduced into each evaporation chamber. It becomes possible to adjust the composition of the compound deposited on the surface of an object.

[実施例] 以下、添附図面を参照して本発明の実施例につ
いて説明する。
[Embodiments] Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings.

図面には本発明による化学蒸着装置の一実施例
を概略的に示し、1は反応室で、その内部には複
数の被蒸着物2を支持する支持部材を成す回転体
3が配置されており、この回転体3は回転軸4を
介して図示してない駆動モータにより制御された
速度で回転駆動される。反応室1の上方部分には
Moを素材としたルツボ5を備えた第1の蒸発室
6およびシリコンを素材としたルツボ7を備えた
第2の蒸発室8が直結されている。第1、第2の
各蒸発室の周囲には高周波加熱コイル9,10が
設けられている。また各蒸発室の上部はそれぞれ
パイプ11,12を介してキヤリアガスボンベ1
3に連結されている。
The drawing schematically shows an embodiment of a chemical vapor deposition apparatus according to the present invention, in which reference numeral 1 denotes a reaction chamber, in which a rotating body 3 serving as a support member for supporting a plurality of objects 2 to be deposited is disposed. This rotating body 3 is rotationally driven via a rotating shaft 4 at a controlled speed by a drive motor (not shown). In the upper part of reaction chamber 1
A first evaporation chamber 6 equipped with a crucible 5 made of Mo and a second evaporation chamber 8 equipped with a crucible 7 made of silicon are directly connected. High frequency heating coils 9 and 10 are provided around each of the first and second evaporation chambers. Further, the upper part of each evaporation chamber is connected to a carrier gas cylinder 1 via pipes 11 and 12, respectively.
It is connected to 3.

第1の蒸発室6のルツボ5にはハロゲン化物の
うちMoCl5が入れられ、また、第2の蒸発室8の
ルツボ9には有機金属のうち(C2H54Siが入れ
られ、これらは室温では固体であるが、それぞれ
高周波加熱コイル9,10により268℃以上およ
び153℃以上に所定温度まで加熱されて気化され
る。
Among the halides, MoCl 5 is placed in the crucible 5 of the first evaporation chamber 6, and (C 2 H 5 ) 4 Si among the organic metals is placed in the crucible 9 of the second evaporation chamber 8. Although these are solid at room temperature, they are heated to predetermined temperatures of 268° C. or higher and 153° C. or higher by high-frequency heating coils 9 and 10, respectively, and are vaporized.

同時に、キヤリアガスボンベ13からは水素ガ
スがパイプ11,12を介して第1、第2の各蒸
発室6,8に対して流量調節されて供給され、各
蒸発室6,8内で気化されたハロゲン化物および
有機金属と一緒に反応室1内の回転体3上の各被
蒸着物2上に導入される。こうして各被蒸着物2
上ではプラズマ反応により金属または金属化合物
が生成され、各被蒸着物2の表面に蒸着して薄膜
が形成される。プラズマ反応により副生されたガ
スおよびキヤリアガスは反応室1に設けた排気口
14から排気される。
At the same time, hydrogen gas was supplied from the carrier gas cylinder 13 via the pipes 11 and 12 to the first and second evaporation chambers 6 and 8 at a controlled flow rate, and was vaporized in each of the evaporation chambers 6 and 8. It is introduced onto each deposition target 2 on the rotating body 3 in the reaction chamber 1 together with the halide and the organic metal. In this way, each deposition target 2
Above, a metal or a metal compound is generated by a plasma reaction, and is deposited on the surface of each deposition target 2 to form a thin film. Gas by-produced by the plasma reaction and carrier gas are exhausted from an exhaust port 14 provided in the reaction chamber 1.

各被蒸着物2の表面に蒸着させる化合物の組成
を例えばMoSi2にしたい場合には、キヤリアガス
の流量を第2の蒸発室8側のキヤリアガスの流量
を第1の蒸発室6側の流量の二倍とし、第2の蒸
発室8側の蒸発ガスの発生速度を第1の蒸発室6
側の蒸発ガスの発生速度の二倍となるように調節
する。
If you want to make the composition of the compound to be vapor-deposited on the surface of each vapor-deposited object 2 to be, for example, MoSi 2 , the flow rate of the carrier gas on the second evaporation chamber 8 side is equal to the flow rate on the first evaporation chamber 6 side. The rate of generation of evaporative gas on the second evaporation chamber 8 side is doubled as that of the first evaporation chamber 6.
Adjust so that the rate of evaporative gas generation on the side is twice as high.

ここで、従来の化学蒸着法では、MoCl5のガス
化に関連して経時変化が若干進行し、このため
MoCl5の他にMoCl4、MoCl3に変化する。その場
合微量ではあるが例えば被蒸着物の表面上に
MoCl4の固体がMoにならずに混入する。このこ
とは、従来の化学蒸着法による装置のように、ハ
ロゲン化部のガス発生装置を系外に設けている場
合には、パイプ等を通過する間に一部MoCl4
MoCl3に経時変化するという機会が多くなること
を意味している。
Here, in the conventional chemical vapor deposition method, there is a slight change over time related to the gasification of MoCl5 , which causes
In addition to MoCl 5 , it changes to MoCl 4 and MoCl 3 . In that case, for example, a small amount may be deposited on the surface of the object to be deposited.
Solid MoCl 4 is mixed in without becoming Mo. This means that when the gas generator for the halogenation section is installed outside the system, as in equipment using conventional chemical vapor deposition, some MoCl 4 and
This means that there will be more opportunities for it to change over time to MoCl 3 .

そこで、本発明に従つてガス発生用の蒸発源を
系内に設けることによつて、純粋なMoCl5ガスを
直接各被蒸着物2の近くに誘導し、プラズマ反応
を行なわせることによりMoとして純粋な薄膜を
形成し蒸着することができる。
Therefore, according to the present invention, by providing an evaporation source for gas generation in the system, pure MoCl 5 gas is directly guided near each deposition target 2, and a plasma reaction is performed to convert it into Mo. Pure thin films can be formed and deposited.

同様にして、Siについても同時に純粋な膜を形
成するが、MoとSiとのモル比が1:2となるよ
うにプラズマ反応を行なうようにすることにより
ClやC等を含まないMoSi2を生成することができ
る。
Similarly, a pure film of Si is also formed at the same time, but by performing a plasma reaction so that the mole ratio of Mo and Si is 1:2.
MoSi 2 that does not contain Cl, C, etc. can be produced.

なお、図示実施例では原料としてMoCl5と(C2
H54Siを用いた例について説明してきたが、当
然他のハロゲン化物や有機金属についても適用で
きる。
In addition, in the illustrated example, MoCl 5 and (C 2
Although we have explained an example using H 5 ) 4 Si, it is of course applicable to other halides and organic metals.

また図示装置では、二つの蒸発室を設けている
が、必要により二つの以上の蒸発室を設けること
もできる。さらに各蒸発室内のルツボを高周波加
熱コイル以外の加熱手段で加熱するようにしても
よい。
Further, although the illustrated apparatus has two evaporation chambers, two or more evaporation chambers may be provided if necessary. Furthermore, the crucible in each evaporation chamber may be heated by heating means other than the high-frequency heating coil.

[発明の効果] 以上説明してきたように、本発明による化学蒸
着装置においては、被蒸着物を収容した反応室に
直結して各蒸発室を設け、しかも蒸発させるべき
材料を入れる容器をその材料を構成している金属
で構成しているので、パイプ系等による不純物の
混入がなく、気化した分子の経時変化がなく、形
成される薄膜の純度や品質を非常に改善させるこ
とができ、また気化した分子が固化することがな
く、装置の操作が容易となり、しかも気化した原
料を通すパイプ等を用いないため装置のメンテナ
ンスが容易となり、経済的である。
[Effects of the Invention] As explained above, in the chemical vapor deposition apparatus according to the present invention, each evaporation chamber is provided directly connected to the reaction chamber containing the material to be evaporated, and the container containing the material to be evaporated is connected directly to the reaction chamber containing the material to be evaporated. Since it is made of metal, there is no contamination by impurities from pipe systems, etc., and there is no change in vaporized molecules over time, making it possible to greatly improve the purity and quality of the thin film formed. The vaporized molecules do not solidify, making it easy to operate the device, and since no pipes or the like are used to pass the vaporized raw material, maintenance of the device is easy and economical.

また、本発明による装置では、各蒸発室に対し
て気化した上記材料の反応室内への流量を制御す
るキヤリアガス供給系を別個に設けているので、
キヤリアガスの流量を調整することによつて被蒸
着物の表面に蒸着される化合物の組成を容易に設
定することができるようになる。
Furthermore, in the apparatus according to the present invention, a carrier gas supply system is separately provided for each evaporation chamber to control the flow rate of the vaporized material into the reaction chamber.
By adjusting the flow rate of the carrier gas, the composition of the compound to be deposited on the surface of the object to be deposited can be easily set.

【図面の簡単な説明】[Brief explanation of the drawing]

図面は本発明による装置の一実施例を概略的に
示す断面図である。 図中、1……反応室、2……被蒸着物、3……
回転体、4……回転軸、5,7……ルツボ、6,
8……蒸発室、9,10……高周波加熱コイル、
11,12……パイプ、13……キヤリアガスボ
ンベ、14……排気口。
The drawing is a sectional view schematically showing an embodiment of the device according to the invention. In the figure, 1... reaction chamber, 2... vapor deposition object, 3...
Rotating body, 4... Rotating shaft, 5, 7... Crucible, 6,
8... Evaporation chamber, 9,10... High frequency heating coil,
11, 12...pipe, 13...carrier gas cylinder, 14...exhaust port.

Claims (1)

【特許請求の範囲】 1 内部に被蒸着物を支持する支持部材を備え、
プラズマ放電により反応を行うようにした反応室
に直結して、複数の蒸発室を設け、各蒸発室に
は、有機金属または金属ハロゲン化物材料を収容
する、それら材料を構成している金属から成る容
器と、上記容器を加熱して上記容器内の化合物を
気化させる加熱手段とを設け、また各蒸発室内の
容器から気化した上記材料の反応室内への流量を
制御するキヤリアガス供給系を各蒸発室に対して
別個に設け、反応室内の上記被蒸着物の表面上に
所望の組成をもつ金属化合物薄膜または単体の金
属薄膜を形成できるように構成したことを特徴と
する化学蒸着装置。 2 被蒸着物を支持する支持部材が反応動作中回
転するようにされた回転体から成る特許請求の範
囲第1項に記載の化学蒸着装置。 3 反応室が反応により副生した排ガスをキヤリ
アガスと共に系外へ排出する排気口を備えている
特許請求の範囲第1項に記載の化学蒸着装置。
[Claims] 1. A support member for supporting an object to be deposited is provided inside,
A plurality of evaporation chambers are provided directly connected to the reaction chamber in which the reaction is carried out by plasma discharge, each evaporation chamber containing an organometallic or metal halide material made of the metal constituting the material. A carrier gas supply system is provided in each evaporation chamber to control the flow rate of the vaporized material from the container in each evaporation chamber into the reaction chamber. 1. A chemical vapor deposition apparatus, characterized in that the chemical vapor deposition apparatus is configured to be provided separately for the vapor deposition target and to form a metal compound thin film or a single metal thin film having a desired composition on the surface of the object to be deposited in the reaction chamber. 2. The chemical vapor deposition apparatus according to claim 1, wherein the support member that supports the object to be deposited comprises a rotating body that rotates during the reaction operation. 3. The chemical vapor deposition apparatus according to claim 1, wherein the reaction chamber is provided with an exhaust port for discharging exhaust gas produced by the reaction to the outside of the system together with a carrier gas.
JP6073086A 1986-03-20 1986-03-20 Chemical vapor deposition method Granted JPS62218574A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP6073086A JPS62218574A (en) 1986-03-20 1986-03-20 Chemical vapor deposition method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6073086A JPS62218574A (en) 1986-03-20 1986-03-20 Chemical vapor deposition method

Publications (2)

Publication Number Publication Date
JPS62218574A JPS62218574A (en) 1987-09-25
JPH0535223B2 true JPH0535223B2 (en) 1993-05-26

Family

ID=13150687

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6073086A Granted JPS62218574A (en) 1986-03-20 1986-03-20 Chemical vapor deposition method

Country Status (1)

Country Link
JP (1) JPS62218574A (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2738017A1 (en) * 1995-08-25 1997-02-28 M3D METHOD FOR COATING A CARBIDE OR A MIXED CARBONITRIDE OF TI AND ZR BY CHEMICAL VAPOR DEPOSITION (CVD) AND DEVICE FOR FORMING A CERAMIC COATING FROM AT LEAST TWO METALLIC PRECURSORS

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4910590A (en) * 1972-05-08 1974-01-30
JPS61194838A (en) * 1985-02-25 1986-08-29 Hitachi Electronics Eng Co Ltd Thin film forming method by cvd and equipment therefor

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4910590A (en) * 1972-05-08 1974-01-30
JPS61194838A (en) * 1985-02-25 1986-08-29 Hitachi Electronics Eng Co Ltd Thin film forming method by cvd and equipment therefor

Also Published As

Publication number Publication date
JPS62218574A (en) 1987-09-25

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