JPH07109576A - Formation of film by plasma cvd - Google Patents

Formation of film by plasma cvd

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Publication number
JPH07109576A
JPH07109576A JP5277897A JP27789793A JPH07109576A JP H07109576 A JPH07109576 A JP H07109576A JP 5277897 A JP5277897 A JP 5277897A JP 27789793 A JP27789793 A JP 27789793A JP H07109576 A JPH07109576 A JP H07109576A
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JP
Japan
Prior art keywords
gas
film
substrate
reaction chamber
undecomposed
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP5277897A
Other languages
Japanese (ja)
Inventor
Shinichi Kobayashi
伸一 小林
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.)
Shinko Seiki Co Ltd
Original Assignee
Shinko Seiki Co Ltd
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 Shinko Seiki Co Ltd filed Critical Shinko Seiki Co Ltd
Priority to JP5277897A priority Critical patent/JPH07109576A/en
Publication of JPH07109576A publication Critical patent/JPH07109576A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To form a thin film having a low content of undecomposed element on the surface of a substrate by plasma CVD. CONSTITUTION:A discharge gas and a raw material decomposing gas are continuously introduced into an evacuated reaction chamber 1, a film forming gas is intermittently introduced by the intermittent opening and closing of piezoelectric valves A and B to be opened and closed by a controller 33, a power is supplied between a substrate 2 and an electrode 3, and the raw material is decomposed. The process of depositing the raw material decomposition product to the surface of the substrate 2 and the process of removing the undecomposed element in the deposit are separately set by the intermittent opening and closing of the piezoelectric valves A and B.

Description

【発明の詳細な説明】Detailed Description of the Invention

【０００１】[0001]

【産業上の利用分野】この発明は基板表面にプラズマＣ
ＶＤ法にて未分解元素の含有率の低い薄膜を形成する方
法に関するものである。This invention relates to plasma C on the surface of a substrate.
The present invention relates to a method for forming a thin film having a low content of undecomposed elements by the VD method.

【０００２】[0002]

【従来の技術】プラズマＣＶＤ法は、化学蒸着法の一種
として被処理物表面への皮膜形成に広く採用されてい
る。このプラズマＣＶＤ法にて基板表面に薄膜を形成さ
せる場合、これまでは原料ガス分解物を基板表面に堆積
させると同時に堆積物中の未分解元素を除去するという
方法で行っている。これは、まず反応室内に導入された
複数の原料ガスを、供給された電力により夫々を構成す
る原子に分解させ、プラズマを発生させ、これら原料ガ
ス分解物が基板に堆積すると同時に熱による表面反応、
ガスやプラズマに曝し、堆積物中の未分解元素を除去す
るというものである。2. Description of the Related Art The plasma CVD method is widely used as a type of chemical vapor deposition method for forming a film on the surface of an object to be processed. In the case of forming a thin film on the surface of a substrate by this plasma CVD method, a method of depositing a decomposed material of a source gas on the surface of the substrate and removing undecomposed elements in the deposited material has hitherto been performed. This is because first of all, a plurality of source gases introduced into the reaction chamber are decomposed by the supplied electric power into the atoms that compose each of them, plasma is generated, and at the same time when these source gas decomposed products are deposited on the substrate, surface reaction by heat is caused. ,
It is to remove undecomposed elements in the deposit by exposing it to gas or plasma.

【０００３】[0003]

【発明が解決しようとする課題】しかしながら、上記の
ような方法の場合、原料ガスを反応室内に連続して導入
しており、基板表面への原料ガス分解物の堆積が連続的
に行われることにより、先に堆積した堆積物中に含まれ
ている未分解元素が完全に除去されないうちに次々とそ
の上に新たな堆積物が積層されていくので、先に堆積し
た堆積物中の未分解元素が含まれたまま成膜が行われる
こととなり、結果的に未分解元素の含有率の高い皮膜が
できやすいという問題があった。However, in the case of the above method, the source gas is continuously introduced into the reaction chamber, and the decomposition products of the source gas are continuously deposited on the substrate surface. As a result, undecomposed elements contained in the previously deposited deposit are not completely removed, and new deposits are successively stacked on top of it, so undecomposed elements in the previously deposited deposit are There is a problem that the film formation is performed with the element contained, and as a result, a film having a high content of undecomposed elements is likely to be formed.

【０００４】この発明は、上記に鑑みて、未分解元素が
除去できて、良質な薄膜を形成することができるプラズ
マＣＶＤによる成膜方法を提供することを目的とするも
のである。In view of the above, it is an object of the present invention to provide a film formation method by plasma CVD capable of removing undecomposed elements and forming a high quality thin film.

【０００５】[0005]

【課題を解決するための手段】即ち、この発明は、排気
された反応室に複数の成膜用原料ガス、放電ガスおよび
原料分解用ガスを導入し、上記反応室に間隔を隔てて設
けた基板と電極との間に電力を供給して、上記原料ガス
を分解させ、上記基板表面に皮膜を形成させるプラズマ
ＣＶＤによる成膜方法において、上記複数の成膜用原料
ガスを間欠的に導入して、基板表面への上記原料ガス分
解物の堆積過程と堆積物中の未分解元素の除去過程とを
別個に設定するとともに、この両過程を周期５秒以下で
繰り返し行うことを特徴とするプラズマＣＶＤによる成
膜方法である。That is, according to the present invention, a plurality of film-forming raw material gases, discharge gas and raw material decomposing gas are introduced into an evacuated reaction chamber and provided in the reaction chamber at intervals. In the film formation method by plasma CVD in which electric power is supplied between the substrate and the electrode to decompose the raw material gas to form a film on the surface of the substrate, the plural raw material gases for film formation are intermittently introduced. And a process of depositing the above-mentioned decomposed material of the source gas on the surface of the substrate and a process of removing undecomposed elements in the deposit are separately set, and both of these processes are repeated at a cycle of 5 seconds or less. This is a film forming method by CVD.

【０００６】[0006]

【作用】プラズマＣＶＤによる成膜方法において、成膜
用原料ガスとしては、化合物を用いる場合が多いが、こ
の化合物の分解を反応室内で完全に行うことは非常に難
しく、このため基板表面に成膜した薄膜中には未分解元
素が残留しやすい。この発明では、複数の成膜用原料ガ
スを間欠的に供給し、これによって基板表面への原料ガ
ス分解物の堆積過程と堆積物中の未分解元素の除去過程
とを成膜工程の１周期内で個々に分けて設定するように
したことで、未分解元素量の少ない薄膜が得られるので
ある。In the film-forming method by plasma CVD, a compound is often used as a film-forming raw material gas, but it is very difficult to completely decompose this compound in the reaction chamber. Undecomposed elements tend to remain in the formed thin film. According to the present invention, a plurality of source gases for film formation are intermittently supplied, whereby the deposition process of the source gas decomposition product on the substrate surface and the removal process of undecomposed elements in the deposition are performed in one cycle of the film formation process. By separately setting the values in the above, a thin film with a small amount of undecomposed elements can be obtained.

【０００７】次に、図１に示すこの発明で使用するプラ
ズマＣＶＤ装置についてその概略を説明する。図におい
て、１は反応室であり、その内部には下方に基板（被処
理物）２が配置され、この基板２に対向するように電極
３が配置されている。この電極３はマッチングボックス
（整合器）５を経て電極４に接続されている。基板２は
その下方に基板加熱用ヒータ６を具えている。また、上
記反応室１は排気系主弁７、ルーツポンプ９を介して油
回転真空ポンプ８に接続されており、この油回転真空ポ
ンプ８の作動によって反応室１内が排気されるようにな
っている。なお、反応室１は、その外周に反応室加熱用
ヒータ１０が取り付けられていて加熱できるようになっ
ている。The plasma CVD apparatus used in the present invention shown in FIG. 1 will be outlined below. In the figure, reference numeral 1 is a reaction chamber, a substrate (object to be processed) 2 is disposed below the reaction chamber, and an electrode 3 is disposed so as to face the substrate 2. The electrode 3 is connected to the electrode 4 via a matching box (matching device) 5. The substrate 2 has a heater 6 for heating the substrate below the substrate 2. The reaction chamber 1 is connected to an oil rotary vacuum pump 8 via an exhaust system main valve 7 and a roots pump 9, and the reaction chamber 1 is exhausted by the operation of the oil rotary vacuum pump 8. ing. A reaction chamber heater 10 is attached to the outer periphery of the reaction chamber 1 so that the reaction chamber 1 can be heated.

【０００８】反応室１には、マスフローコントローラ
（以下、これをＭＦＣという）２１、２２によって流量
を制御されたＨ2 ガス、Ａr ガスがバルブ２５、２６を
介して導入される。また、反応室１には成膜用原料ガス
として、例えばＳｉＨ4 ガスがＭＦＣ２３で流量制御さ
れ、バルブ開閉制御機３３で断続的に開閉されるように
なっているピエゾバルブＡを通って導入される。H 2 gas and Ar gas, the flow rates of which are controlled by mass flow controllers (hereinafter referred to as MFCs) 21 and 22, are introduced into the reaction chamber 1 through valves 25 and 26. Further, for example, SiH 4 gas as a film-forming source gas is introduced into the reaction chamber 1 through a piezo valve A whose flow rate is controlled by the MFC 23 and which is intermittently opened and closed by a valve opening / closing controller 33. .

【０００９】さらに、成膜用原料ガスとして、例えばＴ
ｉＣｌ4 のような常温で液体のものを用いる場合は、容
器３１内にＴｉＣｌ4 を入れ、加熱して気化させてお
き、この気化させた反応ガスを反応室１へ導入する反応
ガス導入管３４にバルブ２９、３０を操作して導き、こ
の反応ガス導入管３４にキャリアガスとして用いるＭＦ
Ｃ２４で流量制御されたＨ2 ガスをバルブ２７、２９、
３０を開閉して供給し、このキャリアＨ2 ガスとともに
反応ガスをバルブ開閉制御機３３で断続的に開閉される
ピエゾバルブＢを経て反応室１内に導入される。この反
応ガスを反応室１内に導入するに当たっては、該ガスが
その供給途中の反応ガス導入管３４内で凝縮するのを防
止するために反応ガス導入管３４はその周囲に取り付け
られた反応ガス導入管加熱用ヒータ３５により加熱され
ることが好ましい。Further, as a film forming source gas, for example, T
When a liquid such as iCl 4 that is liquid at room temperature is used, TiCl 4 is placed in the container 31, heated and vaporized, and the vaporized reaction gas is introduced into the reaction chamber 1 through a reaction gas introduction pipe 34. MF used as a carrier gas for the reaction gas introducing pipe 34 by operating the valves 29, 30 to
The H 2 gas whose flow rate is controlled by C24 is controlled by valves 27, 29,
30 is supplied by opening and closing, and the reaction gas together with the carrier H 2 gas is introduced into the reaction chamber 1 through the piezo valve B which is intermittently opened and closed by the valve opening / closing controller 33. In introducing this reaction gas into the reaction chamber 1, the reaction gas introduction pipe 34 is attached to the periphery of the reaction gas introduction pipe 34 in order to prevent the gas from condensing in the reaction gas introduction pipe 34 during the supply thereof. It is preferably heated by the heater 35 for heating the introduction tube.

【００１０】[0010]

【実施例】次に、上記で説明した図１の装置を用いて、
この発明の実施例を詳細に説明する。 実施例１（珪化チタン膜の作製） まず、反応室１に接続している排気系主弁７を開き、油
回転真空ポンプ８、ルーツポンプ９を作動して反応室１
内を真空排気したのち、反応室加熱用ヒータ１０にて反
応室１内を加熱した。一方、容器３１内に収容されてい
る常温で液体のＴｉＣｌ4 ３２を加熱して気化させる。
同時に気化させたＴｉＣｌ4 ガスを反応室１内に送る反
応ガス導入管３４もその周囲に取り付けた加熱用ヒータ
３５により加熱しておく。次に、反応室１内の基板２を
基板加熱用ヒータ６にて４００℃に加熱した。EXAMPLE Next, using the apparatus of FIG. 1 described above,
Embodiments of the present invention will be described in detail. Example 1 (Production of titanium silicide film) First, the exhaust system main valve 7 connected to the reaction chamber 1 was opened, and the oil rotary vacuum pump 8 and the roots pump 9 were operated to activate the reaction chamber 1.
After evacuating the inside, the reaction chamber 1 was heated by the heater 10 for heating the reaction chamber. On the other hand, liquid TiCl 4 32 contained in the container 31 at normal temperature is heated and vaporized.
At the same time, the reaction gas introduction pipe 34 for sending the vaporized TiCl 4 gas into the reaction chamber 1 is also heated by the heating heater 35 attached to the periphery thereof. Next, the substrate 2 in the reaction chamber 1 was heated to 400 ° C. by the substrate heating heater 6.

【００１１】次いで、加熱され、１５〜２５Ｐａ圧に調
整された反応室１内に夫々ＭＦＣ２１、２２、２３、２
４にて流量制御されたＨ2 ガス、Ａｒガス、ＳｉＨ4 ガ
スと同じく流量制御されたキャリアＨ2 ガスとともに気
化したＴｉＣｌ4 ガスを供給する。この時、Ｈ2 ガス、
Ａｒガスはバルブ２５、２６を開いて連続に供給する。
そして、成膜用原料ガスであるＳｉＨ4 ガスと気化した
ＴｉＣｌ4 ガスの供給は、バルブ開閉制御機３３によっ
て時間的に変化させ、図２に示すように１周期５００ｍ
ｓの間でＴｉＣｌ4 ガスはバルブ２７、２９、３０を開
としてキャリアＨ2 ガスとともに１０ｍｓピエゾパルブ
Ｂを開いて、またＳｉＨ4 ガスは２５０ｍｓピエゾパル
ブＡを開いて供給する。Next, the MFCs 21, 22, 23 and 2 are heated in the reaction chamber 1 adjusted to a pressure of 15 to 25 Pa, respectively.
The vaporized TiCl 4 gas is supplied together with the H 2 gas, the Ar gas, and the SiH 4 gas whose flow rates are controlled at 4, together with the carrier H 2 gas whose flow rate is controlled. At this time, H 2 gas,
Ar gas is continuously supplied by opening the valves 25 and 26.
Then, the supply of the film-forming raw material gas SiH 4 gas and the vaporized TiCl 4 gas is temporally changed by the valve opening / closing controller 33, and as shown in FIG.
During s, the TiCl 4 gas is supplied by opening the valves 27, 29 and 30 to open the piezo valve B for 10 ms together with the carrier H 2 gas, and the SiH 4 gas by opening the piezo valve A for 250 ms.

【００１２】そして、周波数１３．５６ＭＨｚ、１ＫＷ
の容量をもつＲＦ電源４から６００Ｗの電力を反応室１
内に投入する。ここで放電が起こり、電極３と基板２と
の間にプラズマが発生する。このプラズマによって、図
２のようにピエゾパルブＡが開かれている２５０ｍｓの
間は供給されたＴｉＣｌ4 ガス、ＳｉＨ4 ガスが分解さ
れ、基板２表面にＴｉ、Ｓｉが堆積する。その後、ピエ
ゾパルブＡが２５０ｍｓ閉じられると、その間は堆積が
行われず、表面反応によって堆積物中の未分解元素Ｃｌ
を揮発性分子ＨＣｌとして除去する。The frequency of 13.56 MHz, 1 kW
Power of 600W from the RF power source 4 with the capacity of
Throw in. Discharge occurs here and plasma is generated between the electrode 3 and the substrate 2. This plasma decomposes the supplied TiCl 4 gas and SiH 4 gas for 250 ms while the piezo valve A is opened as shown in FIG. 2, and deposits Ti and Si on the surface of the substrate 2. After that, when the piezo pulp A was closed for 250 ms, no deposition was performed during that time, and the undecomposed element Cl in the deposit was caused by the surface reaction.
Is removed as the volatile molecular HCl.

【００１３】このような１周期５００ｍｓによる操作を
１サイクルとして何度も繰り返すことにより、基板２表
面へのＴｉ、Ｓｉの堆積と、堆積物中の未分解元素Ｃｌ
の除去とが図２のように別々の過程で行われることにな
り、基板２表面に未分解元素Ｃｌの含有量の少ない珪化
チタン薄膜が得られる。By repeating such an operation for one cycle of 500 ms as one cycle, Ti and Si are deposited on the surface of the substrate 2 and the undecomposed element Cl in the deposit.
2 is performed in separate steps as shown in FIG. 2, and a titanium silicide thin film having a small content of undecomposed element Cl is obtained on the surface of the substrate 2.

【００１４】かくして得られた珪化チタン薄膜と、原料
ガスを連続的に供給して基板表面への成膜と未分解元素
の除去を同時に行う従来のプラズマＣＶＤ法（以下、従
来法という）にて得た珪化チタン薄膜とについて、Ｘ線
光電子分光分析装置（日本電子社製、ＪＥＳＣＡ−４）
にて膜の組成を分析したところ、この実施例で得た珪化
チタン薄膜中のＣｌ濃度は５％以下であったのに対し、
従来法によるものは１０％以上のＣｌが含まれているこ
とが認められた。そして、これらの珪化チタン薄膜を大
気中に１時間放置したところ、本実施例の珪化チタン薄
膜は何ら異常はなかったが、従来法のものは腐食が起こ
っていた。By the conventional plasma CVD method (hereinafter referred to as a conventional method) in which the titanium silicide thin film thus obtained and the raw material gas are continuously supplied to simultaneously form a film on the substrate surface and remove undecomposed elements. About the obtained titanium silicide thin film, an X-ray photoelectron spectroscopy analyzer (JESCA-4, manufactured by JEOL Ltd.)
When the composition of the film was analyzed by, the Cl concentration in the titanium silicide thin film obtained in this example was 5% or less.
It was confirmed that the conventional method contained 10% or more of Cl. When these titanium silicide thin films were left to stand in the atmosphere for 1 hour, the titanium silicide thin films of this example had no abnormality, but the conventional ones had corrosion.

【００１５】実施例２（窒化珪素膜の作製） 図１の装置を用い、Ａｒガスに代えてＮ2 ガスを用い、
成膜用原料ガスをＳｉＨ4 ガスとＮ2 ガスとした。実施
例１と同様に反応室１内を排気、加熱した後、基板加熱
用ヒータ６にて基板２を２２５℃に加熱した。次いで、
加熱され、１５〜２５Ｐａ圧に調整された反応室１内に
夫々ＭＦＣ２１、２２、２３にて流量制御されたＨ2 ガ
ス、Ｎ2 ガス、ＳｉＨ4 ガスを供給する。この時、Ｈ2
ガスはバルブ２５を開いて連続に供給する。また、成膜
用原料ガスの１つであるＮ2 ガスも放電用ガスでもある
ので、連続的に供給した。そして、もう一方の成膜用原
料ガスであるＳｉＨ4 ガスはバルブ開閉制御機３３によ
って時間的に変化させ、図３に示すように１周期２５０
ｍｓの間で１０ｍｓピエゾパルブＡを開いて供給する。Example 2 (Production of Silicon Nitride Film) Using the apparatus of FIG. 1, N 2 gas was used in place of Ar gas,
The film forming raw material gases were SiH 4 gas and N 2 gas. After exhausting and heating the inside of the reaction chamber 1 in the same manner as in Example 1, the substrate 2 was heated to 225 ° C. by the substrate heating heater 6. Then
The H 2 gas, the N 2 gas, and the SiH 4 gas whose flow rates are controlled by the MFCs 21, 22, and 23 are supplied into the reaction chamber 1 which is heated and adjusted to a pressure of 15 to 25 Pa. At this time, H 2
The gas is supplied continuously by opening the valve 25. Further, N 2 gas, which is one of the film-forming source gases, is also a discharge gas, so it was continuously supplied. Then, the other film forming source gas, SiH 4 gas, is temporally changed by the valve opening / closing controller 33, and as shown in FIG.
Open and supply 10 ms PiezoPalve A between ms.

【００１６】そして、１ＫＷの容量をもつＲＦ電源４か
ら６００Ｗの電力を反応室１内に投入する。ここで放電
が起こり、電極３と基板２との間にプラズマが発生す
る。このプラズマによって、図３のようにピエゾパルブ
Ａが開かれている１０ｍｓから若干の間は供給されたＳ
ｉＨ4 ガス、Ｎ2 ガスが分解され、基板２表面にＳｉ、
Ｎ2 が堆積する。その後、ピエゾパルブＡが閉じられる
と、その間は堆積が行われず、表面反応によって堆積物
中の未分解元素である水素が除去される。Then, 600 W of electric power is supplied to the reaction chamber 1 from the RF power source 4 having a capacity of 1 KW. Discharge occurs here and plasma is generated between the electrode 3 and the substrate 2. As a result of this plasma, as shown in FIG.
iH 4 gas and N 2 gas are decomposed and Si,
N 2 is deposited. After that, when the piezo pulp A is closed, the deposition is not performed during that time, and hydrogen which is an undecomposed element in the deposit is removed by the surface reaction.

【００１７】このような１周期２５０ｍｓによる操作を
１サイクルとして何度も繰り返すことにより、基板２表
面への原料ガス分解物の堆積と、堆積物中の未分解元素
である水素の除去とが別々の過程で行われることにな
り、基板２表面に水素の含有量の少ない窒化珪素の薄膜
が得られる。By repeating this operation for one cycle of 250 ms as one cycle many times, the deposition of the source gas decomposition product on the surface of the substrate 2 and the removal of hydrogen, which is an undecomposed element in the deposition, are separated. As a result of this process, a silicon nitride thin film having a low hydrogen content can be obtained on the surface of the substrate 2.

【００１８】かくして得られた窒化珪素薄膜と、従来法
にて得た窒化珪素薄膜とについて、フーリエ変換赤外分
光装置（日本電子社製、ＪＩＲ−６５００）にて膜中の
水素原子密度を測定したところ、下記表１の結果を得
た。また、本実施例および従来法において、夫々基板温
度を変えて作製した膜についても測定を行った。その結
果、本実施例の膜は従来法にて得た膜より水素原子密度
がかなり低いことがわかった。With respect to the silicon nitride thin film thus obtained and the silicon nitride thin film obtained by the conventional method, the hydrogen atom density in the film was measured by a Fourier transform infrared spectrometer (JIR-6500 manufactured by JEOL Ltd.). Then, the results shown in Table 1 below were obtained. In addition, in the present example and the conventional method, measurement was also performed on films produced by changing the substrate temperature. As a result, it was found that the film of this example had a much lower hydrogen atom density than the film obtained by the conventional method.

【００１９】[0019]

【表１】 [Table 1]

【００２０】実施例３（窒化チタン膜の作製） 図１の装置を用い、ＳｉＨ4 ガスに代えてＮ2 ガスを用
い、成膜用原料ガスをＴｉＣｌ4 ガスとＮ2 ガスとし
た。実施例１と同様に反応室１内を排気、加熱した後、
基板加熱用ヒータ６にて基板２を４００℃に加熱した。
一方容器３１内に収容されている常温で液体のＴｉＣｌ
4 ３２を加熱して気化させる。同時に気化させたＴｉＣ
ｌ4 ガスを反応室１内に送る反応ガス導入管３４も加熱
用ヒータ３５により加熱しておく。Example 3 (Production of Titanium Nitride Film) Using the apparatus shown in FIG. 1, N 2 gas was used instead of SiH 4 gas, and TiCl 4 gas and N 2 gas were used as the film forming source gases. After exhausting and heating the inside of the reaction chamber 1 in the same manner as in Example 1,
The substrate 2 was heated to 400 ° C. by the substrate heating heater 6.
On the other hand, TiCl, which is liquid at room temperature and is contained in the container 31,
4 32 is heated to vaporize. TiC vaporized at the same time
The reaction gas introducing pipe 34 for sending the l 4 gas into the reaction chamber 1 is also heated by the heater 35 for heating.

【００２１】次いで、加熱され、１５〜２５Ｐａ圧に調
整された反応室１内に夫々ＭＦＣ２１、２２、２３，２
４にて流量制御されたＨ2 ガス、Ａｒガス、Ｎ2 ガスお
よび気化したＴｉＣｌ4 ガスを供給する。即ち、Ｈ2 ガ
スおよびＡｒガスはバルブ２５、２６を開いて連続的に
供給する。そして成膜用原料ガスである気化したＴｉＣ
ｌ4 ガスとＮ2 ガスは、夫々のピエゾバルブＢ、Ａの開
閉をバルブ開閉制御機３３によって時間的に変化させて
断続的に供給する。図４に示すように、１周期５００ｍ
ｓの間でまずピエゾバルブＢを１０ｍｓ開き、バルブ２
７、２９、３０を開として導入したキャリアＨ2 ガスと
ともにＴｉＣｌ4 ガスを反応室１内に供給する。Then, the MFCs 21, 22, 23, 2 are respectively heated in the reaction chamber 1 adjusted to a pressure of 15 to 25 Pa.
The H 2 gas, the Ar gas, the N 2 gas, and the vaporized TiCl 4 gas whose flow rates are controlled in 4 are supplied. That is, the H 2 gas and the Ar gas are continuously supplied by opening the valves 25 and 26. And vaporized TiC which is a raw material gas for film formation
The l 4 gas and the N 2 gas are intermittently supplied by changing the opening / closing of the respective piezo valves B and A by the valve opening / closing controller 33 with time. As shown in FIG. 4, one cycle is 500 m
First, open the piezo valve B for 10ms between
TiCl 4 gas is supplied into the reaction chamber 1 together with carrier H 2 gas introduced by opening 7, 29 and 30.

【００２２】そして、１ＫＷの容量をもつＲＦ電源４か
ら６００Ｗの電力を反応室１内に投入する。ここで放電
が起こり、プラズマが発生する。これによって、図４の
ようにＴｉＣｌ4 ガスが分解し、ＣｌがＨＣｌとして除
去される。次いで、バルブ開閉制御機３３によりピエゾ
バルブＡを７５ｍｓ開いて成膜用かつ分解用ガスである
Ｎ2 ガスを反応室１内に供給する。この７５ｍｓの間の
Ｎ2 ガス供給によって反応室１内にＴｉＣｌ4 ガスとＮ
2 ガスが存在する時、これらの原料ガスが分解して基板
２の表面にＴｉＮの堆積が行われる。その後ピエゾバル
ブＡを２５０ｍｓ閉じる（ピエゾバルブＢは既に閉じて
いる）ことにより、堆積は行われず、表面反応によって
堆積物中の未分解元素Ｃｌが除去される。Then, 600 W of electric power is supplied to the reaction chamber 1 from the RF power source 4 having a capacity of 1 KW. Electric discharge occurs here and plasma is generated. As a result, the TiCl 4 gas is decomposed as shown in FIG. 4, and Cl is removed as HCl. Next, the valve opening / closing controller 33 opens the piezo valve A for 75 ms to supply N 2 gas, which is a film forming and decomposition gas, into the reaction chamber 1. By supplying the N 2 gas for 75 ms, TiCl 4 gas and N 2 are fed into the reaction chamber 1.
When two gases are present, these source gases are decomposed and TiN is deposited on the surface of the substrate 2. After that, the piezo valve A is closed for 250 ms (the piezo valve B is already closed), so that the deposition is not performed and the surface reaction removes the undecomposed element Cl in the deposit.

【００２３】このような１周期５００ｍｓによる操作を
１サイクルとして数回繰り返すことにより、ＴｉＮの堆
積と堆積物中の未分解元素Ｃｌの除去とが別々に行わ
れ、基板２表面に未分解元素の含有量の少ないＴｉＮ膜
が得られた。By repeating such an operation for one cycle of 500 ms several times as one cycle, the deposition of TiN and the removal of the undecomposed element Cl in the deposit are carried out separately, and the undecomposed element on the surface of the substrate 2 is removed. A TiN film with a low content was obtained.

【００２４】かくして得られたＴｉＮ膜について、従来
法で得たＴｉＮ膜とともに実施例１と同じ方法で膜の組
成を分析したところ、本実施例のＴｉＮ膜中のＣｌ濃度
は５％以下であったが、従来法によるもののＣｌ濃度は
１０％以上であった。また、これらの膜の大気中１時間
放置で従来法の膜は腐食が見られたが、本実施例の膜は
何らの異常も認められなかった。When the composition of the thus obtained TiN film was analyzed by the same method as in Example 1 together with the TiN film obtained by the conventional method, the Cl concentration in the TiN film of this example was 5% or less. However, the Cl concentration was 10% or more by the conventional method. Further, although the films of the conventional method were found to corrode when these films were left in the atmosphere for 1 hour, no abnormality was observed in the films of this example.

【００２５】実施例４ 図１中のＳｉＨ4 ガスに代えてＯ2 ガスを、またキャリ
アＨ2 ガスに代えてＳｉＨ4 ガスを成膜用原料ガスとし
て用いた。実施例１と同様に反応室１内を排気、加熱し
たのち、基板２を３００℃に加熱した。次いで、１５〜
２５Ｐａ圧にした反応室１内に夫々ＭＦＣ２１、２２、
２３、２４で流量制御されたＨ2 ガス、Ａｒガス、Ｏ2
ガス、ＳｉＨ4 ガスを供給した。このうち、Ｈ2 ガスと
Ａｒガスは連続的に供給した。そして、成膜用原料ガス
のＳｉＨ4 ガスとＯ2 ガスは１周期５００ｍｓの間でピ
エゾバルブＡ、Ｂを図５のように時間的に変化させて開
き、断続的に供給した。The O 2 gas in place of the SiH 4 gas in Example 4 FIG. 1, also using SiH 4 gas in place of the carrier H 2 gas as a film-forming raw material gas. After exhausting and heating the inside of the reaction chamber 1 as in Example 1, the substrate 2 was heated to 300 ° C. Then 15-
In the reaction chamber 1 set to 25 Pa pressure, the MFCs 21 and 22, respectively,
H 2 gas, Ar gas, O 2 whose flow rate is controlled by 23 and 24
Gas and SiH 4 gas were supplied. Of these, H 2 gas and Ar gas were continuously supplied. Then, the SiH 4 gas and the O 2 gas, which are raw material gases for film formation, were intermittently supplied by opening the piezo valves A and B by temporally changing them as shown in FIG. 5 in one cycle of 500 ms.

【００２６】まず、バルブ２７、２８を開としてバルブ
開閉制御機３３にてピエゾバルブＢを１０ｍｓ開いてＳ
ｉＨ4 ガスを反応室１内に供給した。そして、１ＫＷの
容量をもつＲＦ電源４から６００Ｗの電力を反応室１内
に投入する。これによって放電が起こり、プラズマが発
生し、ＳｉＨ4 ガスの分解が起こり、まずＳｉＨ4 の分
解物が基板上に堆積する。その後、堆積したＳｉＨ4 の
分解物中に含まれている未分解元素のＨが除去される。
そして、２５０ｍｓ後にピエゾバルブＢが閉のままバル
ブ開閉制御機３３にてピエゾバルブＡを１０ｍｓ開いて
原料ガスであり、かつ分解用ガスであるＯ2 ガスを供給
する。これによって、その後ピエゾバルブＡ、Ｂが閉と
なっても表面反応によって堆積物とＯ2 等が反応してＳ
ｉＯ2 膜が生成すると同時に堆積物中の未分解元素Ｈを
除去することができる。First, the valves 27 and 28 are opened, the piezo valve B is opened for 10 ms by the valve opening / closing controller 33, and S is set.
iH 4 gas was supplied into the reaction chamber 1. Then, electric power of 600 W is supplied from the RF power source 4 having a capacity of 1 KW into the reaction chamber 1. This causes electric discharge, plasma is generated, SiH 4 gas is decomposed, and first, a decomposed product of SiH 4 is deposited on the substrate. Thereafter, the undecomposed element H contained in the deposited decomposed product of SiH 4 is removed.
After 250 ms, the piezo valve B is closed and the piezo valve A is opened for 10 ms by the valve opening / closing controller 33 to supply O 2 gas which is a raw material gas and a decomposition gas. As a result, even if the piezo valves A and B are subsequently closed, the deposit reacts with O 2 etc. due to the surface reaction, and S
At the same time when the iO 2 film is formed, the undecomposed element H in the deposit can be removed.

【００２７】このような図５に示す５００ｍｓ周期によ
る操作を１サイクルとして数回繰り返すことにより、基
板表面に未分解元素の含有量の少ないＳｉＯ2 膜を形成
することができた。By repeating such an operation with a cycle of 500 ms shown in FIG. 5 as one cycle, a SiO 2 film containing a small amount of undecomposed elements could be formed on the surface of the substrate.

【００２８】これに対して、従来法でＳｉＯ2 膜を形成
しようとすると、原料ガスが連続的に反応室に供給され
るので、反応室内で効率よく原料ガスを分解することが
できず、このため表面に粉が付着したような膜しか得ら
れなかった。On the other hand, when a SiO 2 film is formed by the conventional method, the raw material gas is continuously supplied to the reaction chamber, so that the raw material gas cannot be efficiently decomposed in the reaction chamber. Therefore, only a film with powder adhering to the surface was obtained.

【００２９】上記の実施例においては、プラズマを発生
させる電力を何れも連続的に投入しているが、これは間
欠的投入であってもよい。その電源として周波数１３．
５６ＭＨｚ、容量１ＫＷの電源を用いたが、容量は３０
０Ｗ〜１５ＫＷの範囲を用いることができ、また直流電
源、低周波電源、マイクロ波電源などを用いることもで
き、要するにプラズマ発生手段は限定されない。In the above embodiment, all the electric power for generating plasma is continuously supplied, but this may be intermittent supply. As its power source, frequency 13.
A power source of 56 MHz and a capacity of 1 kW was used, but a capacity of 30
A range of 0 W to 15 KW can be used, and a DC power supply, a low frequency power supply, a microwave power supply, or the like can be used. In short, the plasma generating means is not limited.

【００３０】この発明の成膜方法によれば、上記の実施
例のほか、Ｈ2 ガス、Ａｒガスに成膜用原料ガスとして
ＴｉＣｌ4 とＳｉＣｌ4 を用いて珪化チタン膜を得る場
合、また、Ｈ2 ガス、Ａｒガスに成膜用原料ガスとして
ＳｉＣｌ4 とＣＨ4 を用いて炭化珪素膜を得る場合、さ
らにはＨ2 ガス、Ａｒガスに成膜用原料ガスとして塩化
ホウ素（ＢＣｌ3 、Ｂ2 Ｃｌ4 ）とＮ2 用いて窒化ホウ
素膜を得る場合などにも未分解元素の除去が充分に行え
て夫々良質な膜を得ることができる。According to the film forming method of the present invention, in addition to the above embodiment, when a titanium silicide film is obtained by using TiCl 4 and SiCl 4 as a film forming raw material gas in H 2 gas and Ar gas, When a silicon carbide film is obtained by using SiCl 4 and CH 4 as a film forming raw material gas for H 2 gas and Ar gas, further boron chloride (BCl 3 , B as a film forming raw material gas for H 2 gas and Ar gas). Even when a boron nitride film is obtained using 2 Cl 4 ) and N 2, undecomposed elements can be sufficiently removed, and a good quality film can be obtained.

【００３１】この発明の方法によれば、５００℃以下の
低い基板温度で、しかも膜の堆積過程と堆積物中の未分
解元素の除去過程とを分けることによって未分解元素量
の少ない皮膜を得ることができるので、切削工具や機械
部品の耐摩耗性の向上のために、原料ガスの未分解元素
の含有率が少ない硬質皮膜を６００℃以下の基板温度で
プラズマＣＶＤ法で得る場合や、ＬＳＩなどの電子部品
製造過程で、原料ガスの未分解元素の含有率が少ない導
電性膜、半導体膜、絶縁性膜、バリア膜を６００℃以下
の基板温度でプラズマＣＶＤ法にて得る場合などにこの
発明の成膜方法が有効である。According to the method of the present invention, a film having a small amount of undecomposed elements is obtained at a low substrate temperature of 500 ° C. or lower and by separating the film deposition process and the removal process of undecomposed elements in the deposit. Therefore, in order to improve the wear resistance of cutting tools and machine parts, when a hard coating with a low content of undecomposed elements in the raw material gas is obtained by a plasma CVD method at a substrate temperature of 600 ° C. or lower, In the process of manufacturing electronic components such as, when a conductive film, a semiconductor film, an insulating film, or a barrier film having a low content of undecomposed elements in the source gas is obtained by the plasma CVD method at a substrate temperature of 600 ° C. or less, The film forming method of the invention is effective.

【００３２】[0032]

【発明の効果】以上説明したように、この発明によれ
ば、反応室内に成膜用原料ガス、放電用ガスおよび原料
分解用ガスを導入し、ＲＦ電力を印加して反応室内の基
板表面に薄膜を形成するに際して、成膜用原料ガスの導
入を調整するピエゾバルブの開閉をバルブ開閉制御機に
よって時間的に変化させて断続的に行うこととしたの
で、原料ガス分解物の基板表面への堆積過程と、堆積物
中の未分解元素の除去過程とを別個に設定することがで
き、従って未分解元素の含有量の少ない薄膜を得ること
ができる。As described above, according to the present invention, the film forming material gas, the discharge gas and the material decomposing gas are introduced into the reaction chamber, and RF power is applied to the substrate surface in the reaction chamber. When forming a thin film, it was decided to open and close the piezo valve that regulates the introduction of the raw material gas for film formation intermittently by changing the time with a valve opening / closing controller. The process and the process of removing the undecomposed element in the deposit can be set separately, so that a thin film having a low content of the undecomposed element can be obtained.

【図面の簡単な説明】[Brief description of drawings]

【図１】この発明で使用するプラズマＣＶＤ装置の１例
を示す概略図である。FIG. 1 is a schematic view showing an example of a plasma CVD apparatus used in the present invention.

【図２】実施例１におけるピエゾバルブＡ、Ｂの開閉と
成膜の時間変化を示す説明図である。FIG. 2 is an explanatory diagram showing opening / closing of the piezo valves A and B and time change of film formation in Example 1.

【図３】実施例２におけるピエゾバルブＡの開閉と成膜
の時間変化を示す説明図である。FIG. 3 is an explanatory diagram showing opening / closing of a piezo valve A and time change of film formation in Example 2.

【図４】実施例３におけるピエゾバルブＡ、Ｂの開閉と
成膜の時間変化を示す説明図である。FIG. 4 is an explanatory diagram showing opening / closing of the piezo valves A and B and time change of film formation in Example 3.

【図５】実施例４におけるピエゾバルブＡ、Ｂの開閉と
成膜の時間変化を示す説明図である。FIG. 5 is an explanatory diagram showing opening / closing of piezo valves A and B and time change of film formation in Example 4.

【符号の説明】[Explanation of symbols]

１ 反応室 ２ 基板 ３ 電極 ４ 電源 ３３ バルブ開閉制御機 Ａ ピエゾバルブ Ｂ ピエゾバルブ 1 Reaction chamber 2 Substrate 3 Electrode 4 Power supply 33 Valve open / close controller A Piezo valve B Piezo valve

Claims (1)

【特許請求の範囲】[Claims] 【請求項１】 排気された反応室に複数の成膜用原料ガ
ス、放電ガスおよび原料分解用ガスを導入し、上記反応
室に間隔を隔てて設けた基板と電極との間に電力を供給
して、上記原料ガスを分解させ、上記基板表面に皮膜を
形成させるプラズマＣＶＤによる成膜方法において、上
記複数の成膜用原料ガスを間欠的に導入して、基板表面
への上記原料ガス分解物の堆積過程と堆積物中の未分解
元素の除去過程とを別個に設定するとともに、この両過
程を周期５秒以下で繰り返し行うことを特徴とするプラ
ズマＣＶＤによる成膜方法。1. A plurality of film-forming source gases, a discharge gas and a source-decomposing gas are introduced into an evacuated reaction chamber, and electric power is supplied between a substrate and an electrode provided in the reaction chamber at intervals. Then, in the film forming method by plasma CVD for decomposing the raw material gas and forming a film on the substrate surface, the plural raw material gases for film formation are intermittently introduced to decompose the raw material gas on the substrate surface. A method for forming a film by plasma CVD, characterized in that a deposition process of an object and a removal process of undecomposed elements in the deposit are separately set, and both processes are repeated at a cycle of 5 seconds or less.
JP5277897A 1993-10-07 1993-10-07 Formation of film by plasma cvd Pending JPH07109576A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Publication Number Publication Date
JPH07109576A true JPH07109576A (en) 1995-04-25

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ID=17589816

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Country Link
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WO2003021650A1 (en) * 2001-09-03 2003-03-13 Tokyo Electron Limited Film forming method
WO2004074543A1 (en) * 2003-02-20 2004-09-02 Tokyo Electron Limited Method for forming film
JP2011054968A (en) * 2009-09-03 2011-03-17 Asm Japan Kk METHOD FOR FORMING CONFORMAL DIELECTRIC FILM HAVING Si-N COMBINATION BY PECVD
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