JP2017152672A - Deposition method and deposition system - Google Patents

Deposition method and deposition system Download PDF

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JP2017152672A
JP2017152672A JP2016208128A JP2016208128A JP2017152672A JP 2017152672 A JP2017152672 A JP 2017152672A JP 2016208128 A JP2016208128 A JP 2016208128A JP 2016208128 A JP2016208128 A JP 2016208128A JP 2017152672 A JP2017152672 A JP 2017152672A
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gas
storage
reaction
source gas
film
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JP6675962B2 (en
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侑矢 ▲高▼村
侑矢 ▲高▼村
Yuya Takamura
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Tokyo Electron Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02041—Cleaning
    • H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
    • H01L21/02046—Dry cleaning only
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
    • H01L21/0217—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon nitride not containing oxygen, e.g. SixNy or SixByNz
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
    • H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
    • H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
    • H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H01L21/67028—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like
    • H01L21/67034—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for drying

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Vapour Deposition (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a deposition method capable of depositing a thin film having a desired film thickness distribution.SOLUTION: A deposition method for depositing, on a substrate, a thin film of a reaction product produced by reaction of a material gas and a reaction gas, supplied alternately for the substrate housed in a processing container has a storage step for storing the material gas in a storage section, an adsorption step of supplying the material gas, stored in the storage section to the substrate, and making the substrate adsorb the material gas, and a reaction step of supplying the reaction gas to the substrate that has adsorbed the material gas, and producing the reaction product by causing reaction of the material gas and reaction gas. The storage step, adsorption step, and reaction step are repeated a plurality of times, and the conditions of the storage step are changed at least once while repeating a plurality of times.SELECTED DRAWING: Figure 2

Description

本発明は、成膜方法及び成膜システムに関する。   The present invention relates to a film forming method and a film forming system.

従来、原料ガスと反応ガスとを半導体ウエハ等の基板に対して交互に供給することにより、原料ガスと反応ガスとの反応により生じる反応生成物の薄膜を基板に堆積する方法が知られている。   2. Description of the Related Art Conventionally, a method is known in which a thin film of a reaction product generated by a reaction between a source gas and a reaction gas is deposited on a substrate by alternately supplying a source gas and a reaction gas to a substrate such as a semiconductor wafer. .

また、原料ガスとパージガスとをバッファタンクで混合して混合ガスを生成すると共に混合ガスと反応ガスとを処理容器内へ供給して基板に薄膜を堆積する方法が知られている（例えば、特許文献１参照）。この方法では、成膜レートを高く維持した状態で膜厚の面内均一性を改善している。   Also known is a method of depositing a thin film on a substrate by mixing a source gas and a purge gas in a buffer tank to generate a mixed gas and supplying the mixed gas and a reactive gas into a processing vessel (for example, a patent). Reference 1). In this method, the in-plane uniformity of film thickness is improved while maintaining a high film formation rate.

特開２０１４−００７３７８号公報JP 2014-007378 A

ところで、基板に薄膜を堆積する場合、膜厚の面内均一性が優れていることが必ずしも好ましいとは限らず、所望の膜厚分布を有する薄膜を堆積することが好ましい場合がある。   By the way, when depositing a thin film on a substrate, it is not always preferable that the in-plane uniformity of the film thickness is excellent, and it may be preferable to deposit a thin film having a desired film thickness distribution.

このため、所望の膜厚分布を有する薄膜を堆積することが可能な成膜方法が求められている。   For this reason, a film forming method capable of depositing a thin film having a desired film thickness distribution is required.

上記目的を達成するため、本発明の一態様に係る成膜方法は、原料ガスと反応ガスとを処理容器に収容された基板に対して交互に供給することにより、前記原料ガスと前記反応ガスとの反応により生じる反応生成物の薄膜を前記基板に堆積する成膜方法であって、貯留部に前記原料ガスを貯留する貯留工程と、前記貯留部に貯留された前記原料ガスを前記基板に供給し、前記基板に前記原料ガスを吸着させる吸着工程と、前記原料ガスが吸着した前記基板に前記反応ガスを供給することにより、前記原料ガスと前記反応ガスとを反応させて前記反応生成物を生成する反応工程と、を有し、前記貯留工程と、前記吸着工程と、前記反応工程とを複数回繰り返し、複数回繰り返す間に前記貯留工程の条件を少なくとも１回変更する。   In order to achieve the above object, a film forming method according to one embodiment of the present invention includes supplying a source gas and a reaction gas alternately to a substrate housed in a processing container, whereby the source gas and the reaction gas are supplied. A film forming method for depositing a thin film of a reaction product generated by the reaction with the substrate on the substrate, the storage step storing the source gas in a storage portion, and the source gas stored in the storage portion on the substrate Supplying an adsorption step for adsorbing the source gas on the substrate; and supplying the reaction gas to the substrate on which the source gas is adsorbed to react the source gas with the reaction gas to produce the reaction product The storage step, the adsorption step, and the reaction step are repeated a plurality of times, and the conditions of the storage step are changed at least once while the plurality of times are repeated.

開示の成膜方法によれば、所望の膜厚分布を有する薄膜を堆積することができる。   According to the disclosed film forming method, a thin film having a desired film thickness distribution can be deposited.

本実施形態の成膜装置の一例を示す概略構成図Schematic configuration diagram showing an example of a film forming apparatus of the present embodiment 本実施形態の成膜方法の一例を示すタイミングチャートTiming chart showing an example of a film forming method of the present embodiment ガス流速とウエハ上に堆積するＳｉＮ膜の膜厚分布との関係を説明する図The figure explaining the relationship between the gas flow rate and the film thickness distribution of the SiN film deposited on the wafer ウエハ上にＳｉＮ膜を堆積したときのＳｉＮ膜の特性を示す図（１）The figure which shows the characteristic of a SiN film when depositing a SiN film on a wafer (1) ウエハ上にＳｉＮ膜を堆積したときのＳｉＮ膜の特性を示す図（２）Fig. 2 shows the characteristics of the SiN film when the SiN film is deposited on the wafer. ＤＣＳガスの貯留時間を変化させたときのＳｉＮ膜の特性の変化を説明する図The figure explaining the change of the characteristic of a SiN film when changing the storage time of DCS gas

以下、本発明を実施するための形態について図面を参照して説明する。なお、本明細書及び図面において、実質的に同一の構成については、同一の符号を付することにより重複した説明を省く。   Hereinafter, embodiments for carrying out the present invention will be described with reference to the drawings. In addition, in this specification and drawing, about the substantially same structure, the duplicate description is abbreviate | omitted by attaching | subjecting the same code | symbol.

（成膜装置）
本実施形態の成膜装置の一例について、図１に基づき説明する。図１は、本実施形態の成膜装置の一例を示す概略構成図である。 (Deposition system)
An example of the film forming apparatus of this embodiment will be described with reference to FIG. FIG. 1 is a schematic configuration diagram illustrating an example of a film forming apparatus according to the present embodiment.

図１に示されるように、成膜装置は、長手方向が鉛直方向である略円筒形の処理容器４を有する。処理容器４は、天井を有する外筒６と、外筒６の内側に同心的に配置された円筒体の内筒８とを備える２重管構造を有する。外筒６及び内筒８は、石英等の耐熱性材料により形成されている。外筒６及び内筒８は、ステンレス鋼等から形成されるマニホールド１０によって、その下端部が保持されている。マニホールド１０は、ベースプレート１２に固定されている。なお、マニホールド１０は、外筒６及び内筒８と別部材により形成されているが、構造的には、外筒６及び内筒８と一体的に形成され、外筒６及び内筒８と共に略円筒の内部空間を形成しているため、処理容器４の一部を形成しているものとする。即ち、処理容器４は、石英等の耐熱性材料により形成される外筒６及び内筒８と、ステンレス鋼等により形成されるマニホールド１０とを備え、マニホールド１０は、外筒６及び内筒８を下方から保持するように処理容器４の側面下部に設けられている。   As shown in FIG. 1, the film forming apparatus includes a substantially cylindrical processing container 4 whose longitudinal direction is the vertical direction. The processing container 4 has a double tube structure including an outer cylinder 6 having a ceiling and a cylindrical inner cylinder 8 disposed concentrically inside the outer cylinder 6. The outer cylinder 6 and the inner cylinder 8 are formed of a heat resistant material such as quartz. The lower ends of the outer cylinder 6 and the inner cylinder 8 are held by a manifold 10 formed of stainless steel or the like. The manifold 10 is fixed to the base plate 12. The manifold 10 is formed of a separate member from the outer cylinder 6 and the inner cylinder 8, but is structurally formed integrally with the outer cylinder 6 and the inner cylinder 8, and together with the outer cylinder 6 and the inner cylinder 8. Since a substantially cylindrical internal space is formed, a part of the processing container 4 is formed. That is, the processing container 4 includes an outer cylinder 6 and an inner cylinder 8 formed of a heat resistant material such as quartz, and a manifold 10 formed of stainless steel or the like. The manifold 10 includes the outer cylinder 6 and the inner cylinder 8. Is provided at the lower part of the side surface of the processing container 4 so as to be held from below.

マニホールド１０の下端部の開口部には、例えばステンレス鋼等により形成される円盤状の蓋部１４が、Ｏ−リング等のシール部材１６を介して気密封止可能に取り付けられている。また、蓋部１４の略中心部には、例えば磁性流体シール１８により気密状態を保ちながら回転可能な回転軸２０が挿通されている。回転軸２０の下端は回転機構２２に接続されており、回転軸２０の上端には、例えばステンレス鋼により形成されるテーブル２４が固定されている。   A disk-shaped lid 14 formed of, for example, stainless steel or the like is attached to the opening at the lower end of the manifold 10 through a seal member 16 such as an O-ring so as to be hermetically sealed. Further, a rotating shaft 20 that is rotatable while being kept airtight by a magnetic fluid seal 18 is inserted through a substantially central portion of the lid portion 14. The lower end of the rotating shaft 20 is connected to a rotating mechanism 22, and a table 24 made of, for example, stainless steel is fixed to the upper end of the rotating shaft 20.

テーブル２４上には、例えば石英により形成される保温筒２６が設置されている。また、保温筒２６上には、支持具として例えば石英により形成されるウエハボート２８が載置されている。   On the table 24, a heat insulating cylinder 26 made of, for example, quartz is installed. A wafer boat 28 made of, for example, quartz is mounted on the heat insulating cylinder 26 as a support.

ウエハボート２８は、ウエハＷを処理容器４内で保持するための基板保持手段である。ウエハボート２８には、多数枚（例えば５０〜１７５枚）のウエハＷ等の基板が、所定の間隔、例えば１０ｍｍ程度のピッチで収容される。ウエハボート２８、保温筒２６、テーブル２４及び蓋部１４は、例えばボートエレベータとして機能する昇降機構３０により、処理容器４内に一体となってロード、アンロードされる。   The wafer boat 28 is substrate holding means for holding the wafer W in the processing container 4. In the wafer boat 28, a large number (for example, 50 to 175) of substrates such as wafers W are accommodated at a predetermined interval, for example, a pitch of about 10 mm. The wafer boat 28, the heat retaining cylinder 26, the table 24, and the lid portion 14 are loaded and unloaded integrally in the processing container 4 by, for example, an elevating mechanism 30 that functions as a boat elevator.

また、成膜装置は、処理容器４内へシリコン含有ガス（Ｓｉ含有ガス）を供給するＳｉ含有ガス供給部４０と、処理容器４内へ窒素含有ガスを供給する窒素含有ガス供給部５０と、処理容器４内へパージガスを供給するパージガス供給部６０とを有する。なお、Ｓｉ含有ガスは原料ガスの一例であり、窒素含有ガスは反応ガスの一例である。また、Ｓｉ含有ガス供給部４０は原料ガス供給部の一例であり、窒素含有ガス供給部５０は反応ガス供給部の一例である。   The film forming apparatus includes a Si-containing gas supply unit 40 that supplies a silicon-containing gas (Si-containing gas) into the processing container 4, a nitrogen-containing gas supply unit 50 that supplies a nitrogen-containing gas into the processing container 4, And a purge gas supply unit 60 for supplying a purge gas into the processing container 4. Si-containing gas is an example of a source gas, and nitrogen-containing gas is an example of a reaction gas. The Si-containing gas supply unit 40 is an example of a source gas supply unit, and the nitrogen-containing gas supply unit 50 is an example of a reaction gas supply unit.

Ｓｉ含有ガス供給部４０は、Ｓｉ含有ガス供給源４１と、Ｓｉ含有ガス配管４２と、Ｓｉ含有ガスノズル４３とを有する。   The Si-containing gas supply unit 40 includes a Si-containing gas supply source 41, a Si-containing gas pipe 42, and a Si-containing gas nozzle 43.

Ｓｉ含有ガス配管４２は、Ｓｉ含有ガス供給源４１とＳｉ含有ガスノズル４３とを接続し、Ｓｉ含有ガス供給源４１からのＳｉ含有ガスをＳｉ含有ガスノズル４３へ導く配管である。Ｓｉ含有ガス配管４２には、開閉バルブ４４、流量制御器４５、貯留部（バッファタンク）４６及び開閉バルブ４７が設けられている。例えば開閉バルブ４７を閉じた状態で開閉バルブ４４を開き、Ｓｉ含有ガス供給源４１からＳｉ含有ガスを所定の流量で流すことにより、貯留部４６にＳｉ含有ガスを貯留（チャージ）することができる。貯留部４６にＳｉ含有ガスを貯留した後、開閉バルブ４４を閉じ、開閉バルブ４７を開くことにより、Ｓｉ含有ガスノズル４３を介して所定の量のＳｉ含有ガスを処理容器４内へ供給することができる。   The Si-containing gas pipe 42 is a pipe that connects the Si-containing gas supply source 41 and the Si-containing gas nozzle 43 and guides the Si-containing gas from the Si-containing gas supply source 41 to the Si-containing gas nozzle 43. The Si-containing gas pipe 42 is provided with an opening / closing valve 44, a flow rate controller 45, a reservoir (buffer tank) 46, and an opening / closing valve 47. For example, the Si-containing gas can be stored (charged) in the storage unit 46 by opening the open / close valve 44 with the open / close valve 47 closed and flowing the Si-containing gas from the Si-containing gas supply source 41 at a predetermined flow rate. . After storing the Si-containing gas in the storage section 46, a predetermined amount of Si-containing gas can be supplied into the processing container 4 via the Si-containing gas nozzle 43 by closing the opening / closing valve 44 and opening the opening / closing valve 47. it can.

Ｓｉ含有ガスノズル４３は、Ｓｉ含有ガス配管４２に接続され、マニホールド１０の側壁を内側へと貫通して上方向へ屈曲されて垂直に伸びるノズルであり、例えば石英管により形成されている。Ｓｉ含有ガスノズル４３の垂直部分には、その長さ方向に沿って複数のガス吐出孔４８が所定の間隔で形成されており、各ガス吐出孔４８から水平方向に処理容器４内に向けてほぼ均一にＳｉ含有ガスを吐出することができる。即ち、ウエハＷの表面に平行な方向にＳｉ含有ガスを供給することができる。なお、Ｓｉ含有ガスノズル４３は１本に限らず、２本以上設けられていてもよい。   The Si-containing gas nozzle 43 is a nozzle that is connected to the Si-containing gas pipe 42, penetrates the side wall of the manifold 10 inward, is bent upward, and extends vertically, and is formed of, for example, a quartz tube. In the vertical portion of the Si-containing gas nozzle 43, a plurality of gas discharge holes 48 are formed along the length direction at predetermined intervals, and the gas discharge holes 48 are horizontally directed into the processing container 4 in the horizontal direction. Si-containing gas can be discharged uniformly. That is, the Si-containing gas can be supplied in a direction parallel to the surface of the wafer W. The number of Si-containing gas nozzles 43 is not limited to one, and two or more Si-containing gas nozzles 43 may be provided.

窒素含有ガス供給部５０は、窒素含有ガス供給源５１と、窒素含有ガス配管５２と、窒素含有ガスノズル５３とを有する。   The nitrogen-containing gas supply unit 50 includes a nitrogen-containing gas supply source 51, a nitrogen-containing gas pipe 52, and a nitrogen-containing gas nozzle 53.

窒素含有ガス配管５２は、窒素含有ガス供給源５１と窒素含有ガスノズル５３とを接続し、窒素含有ガス供給源５１からの窒素含有ガスを窒素含有ガスノズル５３へ導く配管である。窒素含有ガス配管５２には、窒素含有ガスの流量を制御する流量制御器５５及び開閉バルブ５７が設けられている。これらにより、窒素含有ガスの供給の開始／停止、及び流量が制御される。   The nitrogen-containing gas pipe 52 is a pipe that connects the nitrogen-containing gas supply source 51 and the nitrogen-containing gas nozzle 53 and guides the nitrogen-containing gas from the nitrogen-containing gas supply source 51 to the nitrogen-containing gas nozzle 53. The nitrogen-containing gas pipe 52 is provided with a flow rate controller 55 and an open / close valve 57 that control the flow rate of the nitrogen-containing gas. Thus, the start / stop of the supply of the nitrogen-containing gas and the flow rate are controlled.

窒素含有ガスノズル５３は、窒素含有ガス配管５２に接続され、マニホールド１０の側壁を内側へ貫通して上方向へ屈曲されて垂直に延びるノズルであり、例えば石英管により形成されている。窒素含有ガスノズル５３の垂直部分には、その長さ方向に沿って複数のガス吐出孔５８が所定の間隔で形成されており、各ガス吐出孔５８から水平方向に処理容器４に向けてほぼ均一に窒素含有ガスを吐出することができる。即ち、ウエハＷの表面に平行な方向に窒素含有ガスを供給することができる。なお、窒素含有ガスノズル５３は１本に限らず、２本以上設けられていてもよい。   The nitrogen-containing gas nozzle 53 is a nozzle that is connected to the nitrogen-containing gas pipe 52, penetrates the side wall of the manifold 10 inward, is bent upward, and extends vertically, and is formed of, for example, a quartz tube. In the vertical portion of the nitrogen-containing gas nozzle 53, a plurality of gas discharge holes 58 are formed at predetermined intervals along the length direction thereof, and are substantially uniform from each gas discharge hole 58 toward the processing container 4 in the horizontal direction. A nitrogen-containing gas can be discharged. That is, the nitrogen-containing gas can be supplied in a direction parallel to the surface of the wafer W. Note that the nitrogen-containing gas nozzle 53 is not limited to one and may be two or more.

パージガス供給部６０は、パージガス供給源６１と、パージガス配管６２と、パージガスノズル６３とを有する。   The purge gas supply unit 60 includes a purge gas supply source 61, a purge gas pipe 62, and a purge gas nozzle 63.

パージガス配管６２は、パージガス供給源６１とパージガスノズル６３とを接続し、パージガス供給源６１からのパージガスをパージガスノズル６３へ導く配管である。パージガス配管６２には、パージガスの流量を制御する流量制御器６５及び開閉バルブ６７が設けられている。これらにより、パージガスの供給の開始／停止、及び流量が制御される。   The purge gas pipe 62 is a pipe that connects the purge gas supply source 61 and the purge gas nozzle 63 and guides the purge gas from the purge gas supply source 61 to the purge gas nozzle 63. The purge gas pipe 62 is provided with a flow rate controller 65 and an open / close valve 67 for controlling the flow rate of the purge gas. Thus, the start / stop of the supply of the purge gas and the flow rate are controlled.

パージガスノズル６３は、パージガス配管６２に接続され、マニホールド１０の側壁を内側へ貫通するストレート形状（直管形状）のノズルであり、例えば石英管により形成されている。   The purge gas nozzle 63 is a straight (straight tube) nozzle that is connected to the purge gas pipe 62 and penetrates the side wall of the manifold 10 to the inside, and is formed of, for example, a quartz tube.

マニホールド１０の上部には、ガス出口３２が設けられており、ガス出口３２には排気系７０が連結されている。排気系７０は、ガス出口３２に接続された排気通路７１と、排気通路７１の途中に順次接続された圧力調整弁７２及び真空ポンプ７３とを含む。排気系７０により、処理容器４内の雰囲気の圧力を調整しながら排気することができる。   A gas outlet 32 is provided in the upper part of the manifold 10, and an exhaust system 70 is connected to the gas outlet 32. The exhaust system 70 includes an exhaust passage 71 connected to the gas outlet 32, and a pressure adjustment valve 72 and a vacuum pump 73 sequentially connected in the middle of the exhaust passage 71. The exhaust system 70 can exhaust while adjusting the pressure of the atmosphere in the processing container 4.

処理容器４の外周側には、処理容器４を囲むようにしてウエハＷを加熱するヒータ装置８０が設けられている。   On the outer peripheral side of the processing container 4, a heater device 80 that heats the wafer W is provided so as to surround the processing container 4.

ヒータ装置８０は、天井面を有する円筒体の断熱層８１を有する。断熱層８１は、例えば熱伝導性が低く、柔らかい無定形のシリカ及びアルミナの混合物によって形成されている。   The heater device 80 includes a cylindrical heat insulating layer 81 having a ceiling surface. The heat insulating layer 81 is formed of, for example, a mixture of soft amorphous silica and alumina having low thermal conductivity.

断熱層８１は、その内周が処理容器４の外面に対して所定の距離だけ離間するように配置される。また、断熱層８１の外周には、ステンレス鋼等により形成される保護カバー８２が、断熱層８１の外周全体を覆うように取り付けられている。   The heat insulating layer 81 is disposed so that the inner periphery thereof is separated from the outer surface of the processing container 4 by a predetermined distance. Further, a protective cover 82 formed of stainless steel or the like is attached to the outer periphery of the heat insulating layer 81 so as to cover the entire outer periphery of the heat insulating layer 81.

断熱層８１の内周側には、ヒータエレメント８３が螺旋状に巻回して配置されている。ヒータエレメント８３は、断熱層８１の内周側に、側面の軸方向全体に亘って巻回して設けられている。   On the inner peripheral side of the heat insulating layer 81, a heater element 83 is spirally wound and disposed. The heater element 83 is provided on the inner peripheral side of the heat insulating layer 81 by being wound over the entire side surface in the axial direction.

ヒータエレメント８３は、軸方向において、複数のゾーン（例えば４つのゾーン）に分割されている。ゾーンごとに断熱層８１に設けられる図示しない熱電対により検出した温度に基づいて、ゾーンごとに独立して温度が制御できる構成となっている。   The heater element 83 is divided into a plurality of zones (for example, four zones) in the axial direction. Based on the temperature detected by the thermocouple which is provided in the heat insulation layer 81 for every zone, it has the structure which can control temperature independently for every zone.

成膜装置の各構成部の制御、例えば開閉バルブ４４、４７、５７、６７の開閉による各ガスの供給／停止、流量制御器４５、５５、６５によるガスの流量の制御、ヒータ装置８０の温度の制御は、コンピュータ等の制御部９０により行われる。   Control of each component of the film forming apparatus, for example, supply / stop of each gas by opening / closing the opening / closing valves 44, 47, 57, 67, control of gas flow rate by the flow rate controllers 45, 55, 65, temperature of the heater device 80 This control is performed by a control unit 90 such as a computer.

制御部９０には、成膜装置で実行される各種処理を制御部９０の制御にて実現するための制御プログラムや、処理条件に応じて成膜装置の各構成部に処理を実行させるための各種のプログラム（又はレシピ）が格納された記憶部９１が接続されている。プログラムには、後述する成膜方法を成膜装置に実行させるプログラムが含まれる。また、各種のプログラムは記憶媒体に記憶され、記憶部９１に格納され得る。記憶媒体は、ハードディスクや半導体メモリであってもよく、ＣＤ−ＲＯＭ、ＤＶＤ、フラッシュメモリ等の可搬性のものであってもよい。また、他の装置から、例えば専用回線を介してレシピを記憶部９１へ適宜伝送させるようにしてもよい。   The control unit 90 has a control program for realizing various processes executed by the film forming apparatus under the control of the control unit 90, and causes each component of the film forming apparatus to execute processes according to processing conditions. A storage unit 91 in which various programs (or recipes) are stored is connected. The program includes a program for causing a film forming apparatus to execute a film forming method to be described later. Various programs can be stored in a storage medium and stored in the storage unit 91. The storage medium may be a hard disk or a semiconductor memory, or may be a portable medium such as a CD-ROM, DVD, or flash memory. Moreover, you may make it transmit a recipe to the memory | storage part 91 suitably from another apparatus, for example via a dedicated line.

（成膜方法）
次に、前述した成膜装置を用いた本実施形態の成膜方法の一例について説明する。 (Film formation method)
Next, an example of the film forming method of the present embodiment using the above-described film forming apparatus will be described.

本実施形態の成膜方法は、Ｓｉ含有ガスと窒素含有ガスとをウエハＷに対して交互に供給することにより、Ｓｉ含有ガスと窒素含有ガスとの反応により生じるシリコン窒化膜（ＳｉＮ膜）をウエハＷ上に堆積するものである。ＳｉＮ膜は、反応生成物の薄膜の一例である。   In the film forming method of this embodiment, a silicon nitride film (SiN film) generated by a reaction between a Si-containing gas and a nitrogen-containing gas is obtained by alternately supplying a Si-containing gas and a nitrogen-containing gas to the wafer W. It is deposited on the wafer W. The SiN film is an example of a thin film of a reaction product.

本実施形態の成膜方法は、貯留工程と、吸着工程と、反応工程とを複数回繰り返し、これらの工程を複数回繰り返す間に、貯留工程の条件を少なくとも１回変更するものである。なお、貯留工程は、貯留部４６にＳｉ含有ガスを貯留する工程である。吸着工程は、貯留部４６に貯留されたＳｉ含有ガスをウエハＷに供給し、ウエハＷにＳｉ含有ガスを吸着させる工程である。反応工程は、Ｓｉ含有ガスが吸着したウエハＷに窒素含有ガスを供給することにより、Ｓｉ含有ガスと窒素含有ガスとを反応させてＳｉＮ膜を生成する工程である。   In the film forming method of this embodiment, the storage process, the adsorption process, and the reaction process are repeated a plurality of times, and the conditions of the storage process are changed at least once while these processes are repeated a plurality of times. The storage step is a step of storing the Si-containing gas in the storage unit 46. The adsorption process is a process in which the Si-containing gas stored in the storage unit 46 is supplied to the wafer W and the Si-containing gas is adsorbed on the wafer W. The reaction step is a step of generating a SiN film by reacting the Si-containing gas and the nitrogen-containing gas by supplying the nitrogen-containing gas to the wafer W on which the Si-containing gas is adsorbed.

以下では、Ｓｉ含有ガスとしてジクロロシラン（ＤＣＳ）ガス、窒素含有ガスとしてアンモニア（ＮＨ３）ガス、パージガスとして窒素（Ｎ２）ガスを用いてＳｉＮ膜を形成する場合を例として挙げ、図２に基づき説明する。図２は、本実施形態の成膜方法の一例を示すタイミングチャートである。図２において、「ＢＦＴ」は貯留部４６の動作を表し、「ＤＣＳ」はＳｉ含有ガス供給部４０の動作を表し、「ＮＨ３」は窒素含有ガス供給部５０の動作を表し、「Ｎ２」はパージガス供給部６０の動作を表す。また、各時刻をｔ１からｔ１１で示す。 In the following, an example in which a SiN film is formed using dichlorosilane (DCS) gas as the Si-containing gas, ammonia (NH 3 ) gas as the nitrogen-containing gas, and nitrogen (N 2 ) gas as the purge gas is shown in FIG. This will be explained based on. FIG. 2 is a timing chart showing an example of the film forming method of the present embodiment. In FIG. 2, “BFT” represents the operation of the storage unit 46, “DCS” represents the operation of the Si-containing gas supply unit 40, “NH 3 ” represents the operation of the nitrogen-containing gas supply unit 50, and “N 2 "Represents the operation of the purge gas supply unit 60. Each time is indicated by t1 to t11.

まず、多数枚のウエハＷが載置された状態のウエハボート２８を予め所定の温度になされた処理容器４内にその下方より上昇させて搬入（ロード）し、蓋部１４でマニホールド１０の下端開口部を閉じることにより処理容器４内を密閉する。続いて、処理容器４内を真空引きし、所定のプロセス圧力に維持すると共に、ヒータ装置８０へ電力を供給することにより、ウエハＷの温度を上昇させてプロセス温度を維持する。また、回転軸２０を回転させることにより、ウエハＷ（ウエハボート２８）を回転させる。   First, the wafer boat 28 on which a large number of wafers W are placed is raised and loaded (loaded) into the processing container 4 that has been set to a predetermined temperature from below, and the lower end of the manifold 10 is covered by the lid 14. The inside of the processing container 4 is sealed by closing the opening. Subsequently, the inside of the processing container 4 is evacuated and maintained at a predetermined process pressure, and power is supplied to the heater device 80 to raise the temperature of the wafer W and maintain the process temperature. Further, by rotating the rotating shaft 20, the wafer W (wafer boat 28) is rotated.

続いて、貯留部４６にＤＣＳガスを貯留する第１の貯留工程を行う。具体的には、図２に示されるように、時刻ｔ１で開閉バルブ４７を閉じた状態で開閉バルブ４４を開き、流量制御器４５により流量を制御しながらＳｉ含有ガス供給源４１から貯留部４６にＤＣＳガスを所定の流量で流し、貯留部４６へのＤＣＳガスの貯留を開始する。このとき、開閉バルブ４７を閉じた状態であるので、ＤＣＳガスが処理容器４内に供給されることはない。所定の貯留時間Ｔ１が経過した後、時刻ｔ２で開閉バルブ４４を閉じ、Ｓｉ含有ガス供給源４１から貯留部４６へのＤＣＳガスの貯留を停止する。所定の貯留時間Ｔ１は、例えば処理容器４の容積、貯留部４６の容積、Ｓｉ含有ガス供給源４１から貯留部４６にＤＣＳガスを流す流量、ウエハＷ上に堆積する膜の膜厚分布に応じて定めることができる。   Then, the 1st storage process which stores DCS gas in storage part 46 is performed. Specifically, as shown in FIG. 2, the opening / closing valve 44 is opened with the opening / closing valve 47 closed at time t <b> 1, and the flow rate controller 45 controls the flow rate while the Si-containing gas supply source 41 supplies the storage unit 46. The DCS gas is allowed to flow at a predetermined flow rate, and the storage of the DCS gas in the storage unit 46 is started. At this time, since the on-off valve 47 is closed, the DCS gas is not supplied into the processing container 4. After the predetermined storage time T1 has elapsed, the opening / closing valve 44 is closed at time t2, and the storage of the DCS gas from the Si-containing gas supply source 41 to the storage unit 46 is stopped. The predetermined storage time T1 depends on, for example, the volume of the processing container 4, the volume of the storage section 46, the flow rate of DCS gas flowing from the Si-containing gas supply source 41 to the storage section 46, and the film thickness distribution of the film deposited on the wafer W. Can be determined.

また、ウエハＷにＮＨ３ガスを供給する反応工程を行う。具体的には、図２に示されるように、貯留工程と同じタイミング（時刻ｔ１）で開閉バルブ５７を開き、流量制御器５５により流量を制御しながら窒素含有ガス供給源５１からＮＨ３ガスを所定の流量で流し、処理容器４内へのＮＨ３ガスの供給を開始する。所定の供給時間Ｔ４が経過した後、時刻ｔ３で開閉バルブ５７を閉じ、窒素含有ガス供給源５１から処理容器４内へのＮＨ３ガスの供給を停止する。所定の供給時間Ｔ４は、吸着工程でウエハＷに吸着したＤＣＳガスを窒化させることが可能な時間であれば特に限定されるものではない。なお、第１のサイクルでは、吸着工程が未だ行われていないため、本工程で反応生成物は生成されないが、第２のサイクル以降では、本工程でＳｉＮ膜が生成される。この点の詳細については後述する。 Also, a reaction process for supplying NH 3 gas to the wafer W is performed. Specifically, as shown in FIG. 2, the opening / closing valve 57 is opened at the same timing (time t1) as the storage process, and the NH 3 gas is supplied from the nitrogen-containing gas supply source 51 while controlling the flow rate by the flow rate controller 55. Flowing at a predetermined flow rate, the supply of NH 3 gas into the processing container 4 is started. After a predetermined supply time T4 has elapsed, the opening / closing valve 57 is closed at time t3, and the supply of NH 3 gas from the nitrogen-containing gas supply source 51 into the processing container 4 is stopped. The predetermined supply time T4 is not particularly limited as long as the DCS gas adsorbed on the wafer W in the adsorption process can be nitrided. In the first cycle, since the adsorption step has not been performed yet, no reaction product is generated in this step, but in the second cycle and thereafter, a SiN film is generated in this step. Details of this point will be described later.

また、図２では、第１の貯留工程が反応工程と同じタイミング（時刻ｔ１）で開始する形態について説明したが、これに限定されるものではない。第１の貯留工程は吸着工程の前に行われていればよく、第１の貯留工程と反応工程とを異なるタイミングで開始してもよいが、１サイクルの時間を短縮できるという観点から、反応工程が行われている期間内に行うことが好ましい。   Moreover, although FIG. 2 demonstrated the form which starts a 1st storage process at the same timing (time t1) as a reaction process, it is not limited to this. The first storage step only needs to be performed before the adsorption step, and the first storage step and the reaction step may be started at different timings. From the viewpoint that the time of one cycle can be shortened, the reaction It is preferable to carry out within the period when the process is performed.

続いて、処理容器４内にＮ２ガスを供給する第１のパージ工程を行う。具体的には、図２に示されるように、時刻ｔ３で開閉バルブ６７を開き、流量制御器６５により流量を制御しながらパージガス供給源６１からＮ２ガスを所定の流量で流し、処理容器４内のＮＨ３ガスのパージを開始する。第１のパージ時間Ｔ５が経過した後、時刻ｔ４で開閉バルブ６７を閉じ、パージガス供給源６１から処理容器４内へのＮ２ガスの供給を停止する。第１のパージ時間Ｔ５は、処理容器４の容積等に応じて定めることができ、例えば１秒から６秒程度とすることができる。なお、図２では、ＮＨ３ガスの供給を停止したタイミングと同じタイミング（時刻ｔ３）で第１のパージ工程を開始しているが、第１のパージ工程を開始するタイミングはこれに限定されるものではない。例えば、第１のパージ工程は、ＮＨ３ガスの供給を停止した後、所定の時間が経過してから開始してもよい。 Subsequently, a first purge step of supplying N 2 gas into the processing container 4 is performed. Specifically, as shown in FIG. 2, the opening / closing valve 67 is opened at time t3, and the N 2 gas is allowed to flow from the purge gas supply source 61 at a predetermined flow rate while controlling the flow rate by the flow rate controller 65. The purge of NH 3 gas inside is started. After the first purge time T5 has elapsed, the open / close valve 67 is closed at time t4, and the supply of N 2 gas from the purge gas supply source 61 into the processing container 4 is stopped. The first purge time T5 can be determined according to the volume of the processing container 4 or the like, and can be set to about 1 to 6 seconds, for example. In FIG. 2, the first purge process is started at the same timing (time t3) as when the supply of NH 3 gas was stopped, but the timing at which the first purge process is started is limited to this. It is not a thing. For example, the first purge process may be started after a predetermined time has elapsed after the supply of NH 3 gas is stopped.

続いて、貯留部４６に貯留されたＤＣＳガスを処理容器４内のウエハＷに供給し、ウエハＷに吸着させる吸着工程を行う。具体的には、図２に示されるように、時刻ｔ４で開閉バルブ４４を閉じ、開閉バルブ４７を開き、貯留部４６に貯留されたＤＣＳガスを処理容器４内へ供給する。所定の供給時間Ｔ３が経過した後、時刻ｔ５で開閉バルブ４７を閉じ、貯留部４６から処理容器４内へのＤＣＳガスの供給を停止する。所定の供給時間Ｔ３は、例えば貯留部４６に貯留されたＤＣＳガスの全量が処理容器４内に供給される時間とすることができる。なお、図２では、Ｎ２ガスの供給を停止したタイミングと同じタイミング（時刻ｔ４）で吸着工程を開始しているが、吸着工程を開始するタイミングはこれに限定されるものではない。例えば、吸着工程は、ＮＨ３ガスの供給を停止した後、所定の時間が経過してから開始してもよい。 Subsequently, an adsorption process is performed in which the DCS gas stored in the storage unit 46 is supplied to the wafer W in the processing container 4 and adsorbed to the wafer W. Specifically, as shown in FIG. 2, the open / close valve 44 is closed and the open / close valve 47 is opened at time t <b> 4 to supply the DCS gas stored in the storage unit 46 into the processing container 4. After the predetermined supply time T3 has elapsed, the opening / closing valve 47 is closed at time t5, and the supply of DCS gas from the storage unit 46 into the processing container 4 is stopped. The predetermined supply time T <b> 3 can be a time during which the entire amount of DCS gas stored in the storage unit 46 is supplied into the processing container 4, for example. In FIG. 2, the adsorption process is started at the same timing (time t4) as when the supply of N 2 gas was stopped, but the timing at which the adsorption process is started is not limited to this. For example, the adsorption process may be started after a predetermined time has elapsed after the supply of NH 3 gas is stopped.

続いて、処理容器４内にＮ２ガスを供給する第２のパージ工程を行う。具体的には、図２に示されるように、時刻ｔ５で開閉バルブ６７を開き、流量制御器６５により流量を制御しながらパージガス供給源６１からＮ２ガスを所定の流量で流し、処理容器４内のＤＣＳガスのパージを開始する。第２のパージ時間Ｔ６が経過した後、時刻ｔ６で開閉バルブ６７を閉じ、パージガス供給源６１から処理容器４内へのＮ２ガスの供給を停止する。第２のパージ時間Ｔ６は、処理容器４の容積等に応じて定めることができ、例えば１秒から６秒程度とすることができる。なお、図２では、ＤＣＳガスの供給を停止したタイミングと同じタイミング（時刻ｔ５）で第２のパージ工程を開始しているが、第２のパージ工程を開始するタイミングはこれに限定されるものではない。例えば、第２のパージ工程は、ＤＣＳガスの供給を停止した後、所定の時間が経過してから開始してもよい。 Subsequently, a second purge step for supplying N 2 gas into the processing container 4 is performed. Specifically, as shown in FIG. 2, the open / close valve 67 is opened at time t5, N 2 gas is allowed to flow from the purge gas supply source 61 at a predetermined flow rate while controlling the flow rate by the flow rate controller 65, and the processing container 4 The purge of the DCS gas inside is started. After the second purge time T6 has elapsed, the open / close valve 67 is closed at time t6, and the supply of N 2 gas from the purge gas supply source 61 into the processing container 4 is stopped. The second purge time T6 can be determined according to the volume of the processing container 4 or the like, and can be set to about 1 to 6 seconds, for example. In FIG. 2, the second purge process is started at the same timing (time t5) as when the supply of DCS gas is stopped, but the timing at which the second purge process is started is limited to this. is not. For example, the second purge process may be started after a predetermined time has elapsed after the supply of DCS gas is stopped.

以上により、第１のサイクルが終了する。   Thus, the first cycle is completed.

次に、第１のサイクルに続いて、第２のサイクルを行う。第２のサイクルでは、第１のサイクルよりも貯留工程におけるＤＣＳガスの貯留時間を長くする。具体的には、図２に示されるように、第１のサイクルにおける貯留工程（第１の貯留工程）の貯留時間Ｔ１と第２のサイクルにおける貯留工程（第２の貯留工程）の貯留時間Ｔ２との関係がＴ１＜Ｔ２となるようにする。   Next, a second cycle is performed following the first cycle. In the second cycle, the DCS gas storage time in the storage process is made longer than in the first cycle. Specifically, as shown in FIG. 2, the storage time T1 of the storage process (first storage process) in the first cycle and the storage time T2 of the storage process (second storage process) in the second cycle. So that T1 <T2.

まず、貯留部４６にＤＣＳガスを貯留する第２の貯留工程を行う。具体的には、図２に示されるように、時刻ｔ６で開閉バルブ４７を閉じた状態で開閉バルブ４４を開き、流量制御器４５により流量を制御しながらＳｉ含有ガス供給源４１からＤＣＳガスを所定の流量で流すことにより、貯留部４６へのＤＣＳガスの貯留を開始する。このとき、開閉バルブ４７を閉じた状態であるので、ＤＣＳガスが処理容器４内に供給されることはない。続いて、第１の貯留工程の貯留時間Ｔ１よりも長い貯留時間Ｔ２が経過した後、時刻ｔ７で開閉バルブ４４を閉じ、Ｓｉ含有ガス供給源４１から貯留部４６へのＤＣＳガスの貯留を停止する。なお、図２では、Ｎ２ガスの供給を停止したタイミングと同じタイミング（時刻ｔ６）で第２の貯留工程を開始しているが、第２の貯留工程を開始するタイミングはこれに限定されるものではない。例えば、第２の貯留工程は、Ｎ２ガスの供給を停止した後、所定の時間が経過してから開始してもよい。 First, the 2nd storage process which stores DCS gas in storage part 46 is performed. Specifically, as shown in FIG. 2, the open / close valve 44 is opened with the open / close valve 47 closed at time t6, and the DCS gas is supplied from the Si-containing gas supply source 41 while controlling the flow rate by the flow rate controller 45. By flowing at a predetermined flow rate, the storage of the DCS gas in the storage unit 46 is started. At this time, since the on-off valve 47 is closed, the DCS gas is not supplied into the processing container 4. Subsequently, after a storage time T2 longer than the storage time T1 of the first storage process has elapsed, the open / close valve 44 is closed at time t7, and storage of DCS gas from the Si-containing gas supply source 41 to the storage unit 46 is stopped. To do. In FIG. 2, the second storage step is started at the same timing (time t6) as when the supply of N 2 gas was stopped, but the timing at which the second storage step is started is limited to this. It is not a thing. For example, the second storage step may be started after a predetermined time has elapsed after the supply of N 2 gas is stopped.

また、ウエハＷにＮＨ３ガスを供給することにより、第１のサイクルの吸着工程でウエハＷ上に吸着しているＤＣＳガスとＮＨ３ガスとを反応させてＳｉＮ膜を生成する反応工程を行う。具体的には、図２に示されるように、貯留工程と同じタイミング（時刻ｔ６）で開閉バルブ５７を開き、窒素含有ガス供給源５１からＮＨ３ガスを所定の流量で流し、処理容器４内へのＮＨ３ガスの供給を開始する。これにより、第１のサイクルの吸着工程でウエハＷ上に吸着しているＤＣＳガスとＮＨ３ガスとを反応させてＳｉＮ膜を生成する。所定の供給時間Ｔ４が経過した後、時刻ｔ８で開閉バルブ５７を閉じ、窒素含有ガス供給源５１から処理容器４内へのＮＨ３ガスの供給を停止する。 Further, by supplying NH 3 gas to the wafer W, a reaction process is performed in which the DCS gas adsorbed on the wafer W in the adsorption process of the first cycle reacts with the NH 3 gas to generate a SiN film. . Specifically, as shown in FIG. 2, the opening / closing valve 57 is opened at the same timing (time t <b> 6) as the storage process, and NH 3 gas is allowed to flow from the nitrogen-containing gas supply source 51 at a predetermined flow rate. The supply of NH 3 gas to is started. As a result, the DCS gas adsorbed on the wafer W in the adsorption process of the first cycle reacts with the NH 3 gas to generate a SiN film. After a predetermined supply time T4 has elapsed, the opening / closing valve 57 is closed at time t8, and the supply of NH 3 gas from the nitrogen-containing gas supply source 51 into the processing container 4 is stopped.

なお、図２では、第２の貯留工程が反応工程と同じタイミング（時刻ｔ６）で開始する形態について説明したが、これに限定されるものではない。第２の貯留工程は吸着工程の前に行われていればよく、第２の貯留工程と反応工程とを異なるタイミングで開始してもよいが、１サイクルの時間を短縮できるという観点から、反応工程が行われている期間内に行うことが好ましい。   In addition, although the form which starts a 2nd storage process at the same timing (time t6) as a reaction process was demonstrated in FIG. 2, it is not limited to this. The second storage step only needs to be performed before the adsorption step, and the second storage step and the reaction step may be started at different timings, but from the viewpoint that the time of one cycle can be shortened. It is preferable to carry out within the period when the process is performed.

続いて、第１のサイクルと同様に、第１のパージ工程、吸着工程及び第２のパージ工程をこの順に行う。   Subsequently, as in the first cycle, the first purge process, the adsorption process, and the second purge process are performed in this order.

具体的には、図２に示されるように、時刻ｔ８で開閉バルブ６７を開き、流量制御器６５により流量を制御しながらパージガス供給源６１からＮ２ガスを所定の流量で流し、処理容器４内のＮＨ３ガスのパージを開始する。第１のパージ時間Ｔ５が経過した後、時刻ｔ９で開閉バルブ６７を閉じ、パージガス供給源６１から処理容器４内へのＮ２ガスの供給を停止する。 Specifically, as shown in FIG. 2, the open / close valve 67 is opened at time t8, and the N 2 gas is allowed to flow from the purge gas supply source 61 at a predetermined flow rate while controlling the flow rate by the flow rate controller 65. The purge of NH 3 gas inside is started. After the first purge time T5 has elapsed, the open / close valve 67 is closed at time t9, and the supply of N 2 gas from the purge gas supply source 61 into the processing container 4 is stopped.

続いて、図２に示されるように、時刻ｔ９で開閉バルブ４４を閉じ、開閉バルブ４７を開き、貯留部４６に貯留されたＤＣＳガスを処理容器４内へ供給する。所定の供給時間Ｔ３が経過した後、時刻ｔ１０で開閉バルブ４７を閉じ、貯留部４６から処理容器４内へのＤＣＳガスの供給を停止する。   Subsequently, as shown in FIG. 2, the opening / closing valve 44 is closed and the opening / closing valve 47 is opened at time t <b> 9, and the DCS gas stored in the storage unit 46 is supplied into the processing container 4. After a predetermined supply time T3 has elapsed, the opening / closing valve 47 is closed at time t10, and the supply of DCS gas from the storage unit 46 into the processing container 4 is stopped.

続いて、図２に示されるように、時刻ｔ１０で開閉バルブ６７を開き、流量制御器６５により流量を制御しながらパージガス供給源６１からＮ２ガスを所定の流量で流し、処理容器４内のＤＣＳガスのパージを開始する。第２のパージ時間Ｔ６が経過した後、時刻ｔ１１で開閉バルブ６７を閉じ、パージガス供給源６１から処理容器４内へのＮ２ガスの供給を停止する。 Subsequently, as shown in FIG. 2, the opening / closing valve 67 is opened at time t10, and N 2 gas is allowed to flow from the purge gas supply source 61 at a predetermined flow rate while controlling the flow rate by the flow rate controller 65. Start purge of DCS gas. After the second purge time T6 has elapsed, the opening / closing valve 67 is closed at time t11, and the supply of N 2 gas from the purge gas supply source 61 into the processing container 4 is stopped.

以上により、第２のサイクルが終了する。   Thus, the second cycle is completed.

以後、第１のサイクルと第２のサイクルとを交互に繰り返すことにより、所望の膜厚を有するＳｉＮ膜を堆積することができる。なお、第１のサイクルと第２のサイクルとを交互に繰り返す際、ウエハＷを処理容器４内に搬入した直後に行われる第１のサイクルでは、ウエハＷにＤＣＳガスが吸着していないため、反応工程を省略してもよい。   Thereafter, an SiN film having a desired film thickness can be deposited by alternately repeating the first cycle and the second cycle. Note that, when the first cycle and the second cycle are alternately repeated, the DCS gas is not adsorbed on the wafer W in the first cycle performed immediately after the wafer W is loaded into the processing container 4. The reaction step may be omitted.

次に、ガス流速とウエハＷ上に堆積するＳｉＮ膜の膜厚分布との関係について、図３に基づき説明する。図３は、ガス流速とウエハ上に堆積するＳｉＮ膜の膜厚分布との関係を説明する図であり、図３（ａ）はガス流速が速い場合を表し、図３（ｂ）はガス流速が遅い場合を表す。   Next, the relationship between the gas flow rate and the film thickness distribution of the SiN film deposited on the wafer W will be described with reference to FIG. 3A and 3B are diagrams for explaining the relationship between the gas flow rate and the thickness distribution of the SiN film deposited on the wafer. FIG. 3A shows the case where the gas flow rate is high, and FIG. 3B shows the gas flow rate. Represents the case where is slow.

貯留工程におけるＤＣＳガスの貯留時間が長い場合、貯留部４６の圧力が高くなるため、吸着工程において貯留部４６から処理容器４内へ供給されるＤＣＳガスの流速が速くなる。このため、図３（ａ）に示されるように、Ｓｉ含有ガスノズル４３から供給されるＤＣＳガスの温まりが遅く、ウエハＷの外周部領域よりも中央部領域においてＤＣＳガスが吸着しやすい状態となる。その結果、ウエハＷ上に堆積するＳｉＮ膜は、ウエハＷの外周部領域から中央部領域に向けて膜厚が厚くなる分布となる。   When the storage time of the DCS gas in the storage process is long, the pressure of the storage part 46 increases, and thus the flow rate of the DCS gas supplied from the storage part 46 into the processing container 4 in the adsorption process increases. For this reason, as shown in FIG. 3A, the warming of the DCS gas supplied from the Si-containing gas nozzle 43 is slow, and the DCS gas is more easily adsorbed in the central region than in the outer peripheral region of the wafer W. . As a result, the SiN film deposited on the wafer W has a distribution in which the film thickness increases from the outer peripheral region to the central region of the wafer W.

これに対して、貯留工程における貯留時間が短い場合、貯留部４６の圧力が低くなるため、吸着工程において貯留部４６から処理容器４内へ供給されるＤＣＳガスの流速が遅くなる。このため、図３（ｂ）に示されるように、Ｓｉ含有ガスノズル４３から供給されるＤＣＳガスの温まりが速く、ウエハＷの外周部領域及び中央部領域でＤＣＳガスが吸着しやすい状態となる。その結果、ウエハＷ上に堆積するＳｉＮ膜は、ウエハＷの外周部領域から中央部領域まで略均一の膜厚分布となる。   On the other hand, when the storage time in the storage process is short, the pressure of the storage part 46 is lowered, and thus the flow rate of the DCS gas supplied from the storage part 46 into the processing container 4 in the adsorption process is slow. For this reason, as shown in FIG. 3B, the DCS gas supplied from the Si-containing gas nozzle 43 is warmed up so that the DCS gas is easily adsorbed in the outer peripheral region and the central region of the wafer W. As a result, the SiN film deposited on the wafer W has a substantially uniform film thickness distribution from the outer peripheral region to the central region of the wafer W.

本実施形態では、前述したように、貯留工程におけるＤＣＳガスの貯留時間が異なる第１のサイクルと第２のサイクルとを交互に繰り返す。これにより、第１のサイクルで得られるＳｉＮ膜の膜厚分布と、第２のサイクルで得られるＳｉＮ膜の膜厚分布とを組み合わせた膜厚分布を有するＳｉＮ膜を堆積することができる。また、第１のサイクルにおける貯留工程（第１の貯留工程）の貯留時間Ｔ１と第２のサイクルにおける貯留工程（第２の貯留工程）の貯留時間Ｔ２とを調整することで、容易に所望の膜厚分布を有する薄膜を堆積することができる。   In the present embodiment, as described above, the first cycle and the second cycle with different DCS gas storage times in the storage step are alternately repeated. Thereby, a SiN film having a thickness distribution obtained by combining the thickness distribution of the SiN film obtained in the first cycle and the thickness distribution of the SiN film obtained in the second cycle can be deposited. Further, by adjusting the storage time T1 of the storage process (first storage process) in the first cycle and the storage time T2 of the storage process (second storage process) in the second cycle, the desired time can be easily obtained. A thin film having a film thickness distribution can be deposited.

なお、本実施形態では、第１の貯留工程と第２の貯留工程とにおける貯留時間が異なる場合について説明したが、係る形態に限定されるものではない。第１の貯留工程と第２の貯留工程とは、貯留部４６にＤＣＳガスを貯留したときの貯留部４６の圧力が異なっていればよく、例えばＳｉ含有ガス供給源４１から貯留部４６にＤＣＳガスを貯留する際のＤＣＳガスの流量が異なっていてもよい。また、貯留時間とＤＣＳガスの流量との両方が異なるようにしてもよい。   In addition, although this embodiment demonstrated the case where the storage time in a 1st storage process and a 2nd storage process differs, it is not limited to the form which concerns. The first storage step and the second storage step only need to have different pressures in the storage unit 46 when DCS gas is stored in the storage unit 46. For example, the DCS is supplied from the Si-containing gas supply source 41 to the storage unit 46. The flow rate of the DCS gas when storing the gas may be different. Further, both the storage time and the flow rate of the DCS gas may be different.

（実施例）
次に、成膜方法の具体的な例について、図４に基づき説明する。図４はウエハ上にＳｉＮ膜を堆積したときのＳｉＮ膜の特性を示す図であり、図４（ａ）はウエハの面内における膜厚分布を表し、図４（ｂ）は１サイクルあたりの成膜速度及び膜厚の面内均一性を表す。図４（ｂ）における棒グラフは１サイクルあたりの成膜速度を表し、折れ線グラフは膜厚の面内均一性を表す。 (Example)
Next, a specific example of the film forming method will be described with reference to FIG. FIG. 4 is a diagram showing the characteristics of the SiN film when the SiN film is deposited on the wafer. FIG. 4A shows the film thickness distribution in the plane of the wafer, and FIG. In-plane uniformity of film formation speed and film thickness. The bar graph in FIG. 4B represents the film formation rate per cycle, and the line graph represents the in-plane uniformity of the film thickness.

本実施例では、いずれの条件においても貯留工程と、吸着工程と、反応工程とを含むサイクルを複数回繰り返すことで、ウエハＷ上にＳｉＮ膜を堆積した。また、ウエハボート２８には多数枚のウエハＷを保持させ、高さ方向に５つの領域に区分して、その上方から下方に向けて「ＴＯＰ」、「ＴＣ」、「ＣＴＲ」、「ＣＢ」及び「ＢＴＭ」としてそれぞれの領域におけるＳｉＮ膜の特性を評価した。図４（ａ）は「ＴＯＰ」、「ＣＴＲ」及び「ＢＴＭ」における膜厚分布を表し、図４（ｂ）は「ＴＯＰ」、「ＴＣ」、「ＣＴＲ」、「ＣＢ」及び「ＢＴＭ」における１サイクルあたりの成膜速度及び膜厚の面内均一性を表す。   In this example, the SiN film was deposited on the wafer W by repeating the cycle including the storage process, the adsorption process, and the reaction process a plurality of times under any conditions. The wafer boat 28 holds a large number of wafers W, is divided into five regions in the height direction, and "TOP", "TC", "CTR", "CB" from above to below. The characteristics of the SiN film in each region were evaluated as “BTM”. 4A shows the film thickness distribution in “TOP”, “CTR”, and “BTM”, and FIG. 4B shows the film thickness distribution in “TOP”, “TC”, “CTR”, “CB”, and “BTM”. In-plane uniformity of film formation rate and film thickness per cycle.

また、図４（ａ）及び図４（ｂ）における最も左側の図はＤＣＳガスの流量をｘ（ｓｌｍ）、貯留（ＣＨＧ）時間をＴ１１（秒）としたとき（第１の貯留条件）のＳｉＮ膜の特性を表す。また、左側から２番目の図はＤＣＳガスの流量をｘ（ｓｌｍ）、貯留（ＣＨＧ）時間をＴ１２（秒）としたとき（第２の貯留条件）のＳｉＮ膜の特性を表す。なお、Ｔ１１＜Ｔ１２である。また、左側から３番目の図は第１の貯留条件を用いた場合のＳｉＮ膜の特性及び第２の貯留条件を用いた場合のＳｉＮ膜の特性に基づいて、第１の貯留条件の貯留工程と第２の貯留条件の貯留工程とを交互に繰り返したときのＳｉＮ膜の特性をシミュレーションにより予測した結果を表す。さらに、最も右側の図は第１の貯留条件の貯留工程と第２の貯留条件の貯留工程とを交互に繰り返したときのＳｉＮ膜の特性を実測した結果を表す。   4 (a) and 4 (b) are the leftmost diagrams when the flow rate of DCS gas is x (slm) and the storage (CHG) time is T11 (seconds) (first storage condition). It represents the characteristics of the SiN film. The second diagram from the left represents the characteristics of the SiN film when the flow rate of DCS gas is x (slm) and the storage (CHG) time is T12 (second storage condition) (second storage condition). Note that T11 <T12. The third drawing from the left shows the storage process of the first storage condition based on the characteristics of the SiN film when the first storage condition is used and the characteristics of the SiN film when the second storage condition is used. The result of having predicted the characteristic of the SiN film | membrane by simulation when repeating the storage process of 2nd and storage conditions alternately is represented. Further, the rightmost diagram shows the result of actually measuring the characteristics of the SiN film when the storage process of the first storage condition and the storage process of the second storage condition are alternately repeated.

図４（ａ）及び図４（ｂ）に示されるように、第１の貯留条件の貯留工程と第２の貯留条件の貯留工程とを交互に繰り返したときのＳｉＮ膜の膜厚分布、１サイクルあたりの成膜速度及び膜厚の面内均一性について、シミュレーションにより算出した結果（左から３番目の図）と実測した結果（最も右側の図）とが略同一の結果となっていることが分かる。即ち、互いに異なる２つの貯留条件の貯留工程を交互に繰り返すことにより得られるＳｉＮ膜の特性を予測することができる。これにより、互いに異なる貯留条件の貯留工程を交互に繰り返すことで、ウエハＷ上に堆積するＳｉＮ膜の膜厚分布、１サイクルあたりの成膜速度及び膜厚の面内均一性を制御することができる。   As shown in FIGS. 4A and 4B, the film thickness distribution of the SiN film when the storage process of the first storage condition and the storage process of the second storage condition are alternately repeated, Regarding the film formation rate per cycle and the in-plane uniformity of film thickness, the results calculated by simulation (the third figure from the left) and the measured results (the rightmost figure) are substantially the same. I understand. That is, it is possible to predict the characteristics of the SiN film obtained by alternately repeating storage processes under two different storage conditions. Thereby, by alternately repeating storage processes under different storage conditions, the film thickness distribution of the SiN film deposited on the wafer W, the film formation speed per cycle, and the in-plane uniformity of the film thickness can be controlled. it can.

次に、成膜方法の他の具体的な例について、図５に基づき説明する。図５はウエハ上にＳｉＮ膜を堆積したときのＳｉＮ膜の特性を示す図であり、図５（ａ）はウエハの面内における膜厚分布を表し、図５（ｂ）は１サイクルあたりの成膜速度及び膜厚の面内均一性を表す。図５（ｂ）における棒グラフは１サイクルあたりの成膜速度を表し、折れ線グラフは膜厚の面内均一性を表す。   Next, another specific example of the film forming method will be described with reference to FIG. FIG. 5 is a diagram showing the characteristics of the SiN film when the SiN film is deposited on the wafer. FIG. 5A shows the film thickness distribution in the plane of the wafer, and FIG. In-plane uniformity of film formation speed and film thickness. The bar graph in FIG. 5B represents the film formation rate per cycle, and the line graph represents the in-plane uniformity of the film thickness.

本実施例では、いずれの条件においても貯留工程と、吸着工程と、反応工程とを含むサイクルを複数回繰り返すことで、ウエハＷ上にＳｉＮ膜を堆積した。また、ウエハボート２８には多数枚のウエハＷを保持させ、高さ方向に５つの領域に区分して、その上方から下方に向けて「ＴＯＰ」、「ＴＣ」、「ＣＴＲ」、「ＣＢ」及び「ＢＴＭ」としてそれぞれの領域におけるＳｉＮ膜の特性を評価した。図５（ａ）は「ＴＯＰ」、「ＣＴＲ」及び「ＢＴＭ」における膜厚分布を表し、図５（ｂ）は「ＴＯＰ」、「ＴＣ」、「ＣＴＲ」、「ＣＢ」及び「ＢＴＭ」における１サイクルあたりの成膜速度及び膜厚の面内均一性を表す。   In this example, the SiN film was deposited on the wafer W by repeating the cycle including the storage process, the adsorption process, and the reaction process a plurality of times under any conditions. The wafer boat 28 holds a large number of wafers W, is divided into five regions in the height direction, and "TOP", "TC", "CTR", "CB" from above to below. The characteristics of the SiN film in each region were evaluated as “BTM”. 5A shows the film thickness distribution in “TOP”, “CTR” and “BTM”, and FIG. 5B shows the film thickness distribution in “TOP”, “TC”, “CTR”, “CB” and “BTM”. In-plane uniformity of film formation rate and film thickness per cycle.

また、図５（ａ）及び図５（ｂ）における左側の図はＤＣＳガスの流量をｙ（ｓｌｍ）、貯留（ＣＨＧ）時間をＴ１３（秒）としたとき（第３の貯留条件）のＳｉＮ膜の特性を表す。また、中央の図はＤＣＳガスの流量をｙ（ｓｌｍ）、貯留（ＣＨＧ）時間をＴ１４（秒）としたとき（第４の貯留条件）のＳｉＮ膜の特性を表す。なお、Ｔ１３＜Ｔ１４である。また、右側の図は第３の貯留条件を用いた場合のＳｉＮ膜の特性及び第４の貯留条件を用いた場合のＳｉＮ膜の特性に基づいて、第３の貯留条件の貯留工程と第４の貯留条件の貯留工程とを交互に繰り返したときのＳｉＮ膜の特性をシミュレーションにより予測した結果を表す。   5 (a) and 5 (b), the diagrams on the left side show SiN when the flow rate of DCS gas is y (slm) and the storage (CHG) time is T13 (second) (third storage condition). Represents the characteristics of the membrane. The center diagram shows the characteristics of the SiN film when the flow rate of DCS gas is y (slm) and the storage (CHG) time is T14 (second storage condition) (fourth storage condition). Note that T13 <T14. Further, the right side diagram shows the storage process of the third storage condition and the fourth based on the characteristics of the SiN film when the third storage condition is used and the characteristics of the SiN film when the fourth storage condition is used. The result of having predicted the characteristic of the SiN film | membrane by simulation when repeating the storage process of these storage conditions alternately is represented.

図５（ａ）及び図５（ｂ）に示されるように、シミュレーションにより第１の貯留条件の貯留工程と第２の貯留条件の貯留工程とを交互に繰り返したときのＳｉＮ膜の膜厚分布、１サイクルあたりの成膜速度及び膜厚の面内均一性を予測することができる。これにより、互いに異なる貯留条件の貯留工程を交互に繰り返すことで、ウエハＷ上に堆積するＳｉＮ膜の膜厚分布、１サイクルあたりの成膜速度及び膜厚の面内均一性を制御することができる。   As shown in FIGS. 5A and 5B, the thickness distribution of the SiN film when the storage process of the first storage condition and the storage process of the second storage condition are alternately repeated by simulation. The film formation rate per cycle and the in-plane uniformity of film thickness can be predicted. Thereby, by alternately repeating storage processes under different storage conditions, the film thickness distribution of the SiN film deposited on the wafer W, the film formation speed per cycle, and the in-plane uniformity of the film thickness can be controlled. it can.

次に、貯留工程におけるＤＣＳガスの貯留時間を変化させたときのＳｉＮ膜の膜厚分布、１サイクルあたりの成膜速度及び膜厚の面内均一性について、図６に基づき説明する。図６はＤＣＳガスの貯留時間を変化させたときのＳｉＮ膜の特性の変化を説明する図であり、図６（ａ）はウエハの面内における膜厚分布を表し、図６（ｂ）は１サイクルあたりの成膜速度及び膜厚の面内均一性を表す。図６（ｂ）における棒グラフは１サイクルあたりの成膜速度を表し、折れ線グラフは膜厚の面内均一性を表す。   Next, the film thickness distribution of the SiN film when the DCS gas storage time in the storage process is changed, the film formation speed per cycle, and the in-plane uniformity of the film thickness will be described with reference to FIG. FIG. 6 is a diagram for explaining changes in the characteristics of the SiN film when the DCS gas storage time is changed. FIG. 6A shows the film thickness distribution in the plane of the wafer, and FIG. In-plane uniformity of film formation rate and film thickness per cycle. The bar graph in FIG. 6B represents the film formation rate per cycle, and the line graph represents the in-plane uniformity of the film thickness.

また、図６（ａ）及び図６（ｂ）においては、左側の図から順に、ＤＣＳガスの貯留（ＣＨＧ）時間を１０秒、１２秒、１４秒、１６秒、１８秒とした場合の結果を示している。   6 (a) and 6 (b), the results when the DCS gas storage (CHG) time is 10 seconds, 12 seconds, 14 seconds, 16 seconds, and 18 seconds in order from the left side of the figure. Is shown.

図６（ａ）に示されるように、ＤＣＳガスの貯留時間を長くするほど、中央部領域と外周部領域との膜厚の差が大きくなることが分かる。また、図６（ｂ）に示されるように、ＤＣＳガスの貯留時間を長くするほど、１サイクルあたりの成膜速度及び膜厚の面内均一性の値が大きくなることが分かる。即ち、ＤＣＳガスの貯留時間を調整することにより、ウエハＷ上に堆積するＳｉＮ膜の膜厚分布、１サイクルあたりの成膜速度及び膜厚の面内均一性を制御することができる。   As shown in FIG. 6A, it can be seen that the longer the DCS gas storage time, the greater the difference in film thickness between the central region and the peripheral region. Further, as shown in FIG. 6B, it can be seen that the longer the DCS gas storage time, the larger the film formation rate per cycle and the in-plane uniformity value of the film thickness. That is, by adjusting the storage time of the DCS gas, the film thickness distribution of the SiN film deposited on the wafer W, the film formation speed per cycle, and the in-plane uniformity of the film thickness can be controlled.

以上、成膜方法を上記実施形態により説明したが、本発明は上記実施形態に限定されるものではなく、本発明の範囲内で種々の変形及び改良が可能である。   As described above, the film forming method has been described by the above embodiment, but the present invention is not limited to the above embodiment, and various modifications and improvements can be made within the scope of the present invention.

本実施形態では、原料ガスとしてＳｉ含有ガスであるＤＣＳガスを用いたが、本発明はこれに限定されるものではない。Ｓｉ含有ガスとしては、例えばジクロロシラン（ＤＣＳ）、ヘキサクロロジシラン（ＨＣＤ）、モノシラン（ＳｉＨ４）、ジシラン（Ｓｉ２Ｈ６）、ヘキサメチルジシラザン（ＨＭＤＳ）、テトラクロロシラン（ＴＣＳ）、ジシリルアミン（ＤＳＡ）、トリシリルアミン（ＴＳＡ）、ビスターシャルブチルアミノシラン（ＢＴＢＡＳ）、ビスジエチルアミノシラン（ＢＤＥＡＳ）、ジイソプロピルアミノシラン（ＤＩＰＡＳ）、トリスジメチルアミノシラン（３ＤＭＡＳ）よりなる群より選択される１以上のガスを用いることができる。 In this embodiment, the DCS gas that is a Si-containing gas is used as the raw material gas, but the present invention is not limited to this. Examples of the Si-containing gas include dichlorosilane (DCS), hexachlorodisilane (HCD), monosilane (SiH 4 ), disilane (Si 2 H 6 ), hexamethyldisilazane (HMDS), tetrachlorosilane (TCS), and disilylamine (DSA). ), Trisilylamine (TSA), binary butylaminosilane (BTBAS), bisdiethylaminosilane (BDEAS), diisopropylaminosilane (DIPAS), and trisdimethylaminosilane (3DMAS). Can do.

また、反応ガスとして窒素含有ガスであるＮＨ３ガスを用いたが、本発明はこれに限定されるものではない。窒素含有ガスとしては、例えば一酸化二窒素（Ｎ２Ｏ）、一酸化窒素（ＮＯ）を用いることができる。さらに、反応ガスとして、窒素含有ガスに代えて酸素含有ガスを用いることもできる。 Further, NH 3 is used gas is a nitrogen-containing gas as a reaction gas, the present invention is not limited thereto. As the nitrogen-containing gas, for example, dinitrogen monoxide (N 2 O) or nitric oxide (NO) can be used. Further, an oxygen-containing gas can be used as the reaction gas instead of the nitrogen-containing gas.

また、本実施形態では、原料ガスとしてＳｉ含有ガス、反応ガスとして窒素含有ガスを用いてＳｉＮ膜を堆積する場合を例として説明したが、本発明はこれに限定されるものではない。原料ガスとして金属を含む金属化合物ガスを用いて金属窒化膜や金属酸化膜等を堆積するようにしてもよい。金属化合物ガスとしては、例えば有機金属化合物ガスを用いることができ、例えばトリメチルアルミニウム（ＴＭＡ）、テトラキスジメチルアミノハフニウム（ＴＤＭＡＨ）、テトラキスエチルメチルアミノハフニウム（ＴＥＭＡＨ）、テトラキスエチルメチルアミノジルコニウム（ＴＥＭＡＺ）、テトラキスジメチルアミノチタン（ＴＤＭＡＴ）よりなる群より選択される１以上のガスを用いることができる。   In the present embodiment, the SiN film is deposited using Si-containing gas as the source gas and nitrogen-containing gas as the reaction gas. However, the present invention is not limited to this. A metal nitride film or a metal oxide film may be deposited using a metal compound gas containing a metal as a source gas. As the metal compound gas, for example, an organometallic compound gas can be used. For example, trimethylaluminum (TMA), tetrakisdimethylaminohafnium (TDMAH), tetrakisethylmethylaminohafnium (TEMAH), tetrakisethylmethylaminozirconium (TEMAZ), One or more gases selected from the group consisting of tetrakisdimethylaminotitanium (TDMAT) can be used.

また、本実施形態では、基板として半導体ウエハを例として説明したが、この半導体ウエハにはシリコン基板、ＧａＡｓ、ＳｉＣ、ＧａＮ等の化合物半導体基板も含まれ、更にはこれらの基板に限定されず、液晶表示装置に用いるガラス基板やセラミック基板等にも本発明を適用することができる。   In the present embodiment, the semiconductor wafer is described as an example of the substrate. However, the semiconductor wafer includes a compound semiconductor substrate such as a silicon substrate, GaAs, SiC, and GaN, and is not limited to these substrates. The present invention can also be applied to a glass substrate, a ceramic substrate, or the like used in a liquid crystal display device.

４ 処理容器
４０ Ｓｉ含有ガス供給部
４１ Ｓｉ含有ガス供給源
４２ Ｓｉ含有ガス配管
４３ Ｓｉ含有ガスノズル
４４ 開閉バルブ
４５ 流量制御器
４６ 貯留部
４７ 開閉バルブ
４８ ガス吐出孔
５０ 窒素含有ガス供給部
５１ 窒素含有ガス供給源
５２ 窒素含有ガス配管
５３ 窒素含有ガスノズル
５５ 流量制御器
５７ 開閉バルブ
５８ ガス吐出孔
６０ パージガス供給部
６１ パージガス供給源
６２ パージガス配管
６３ パージガスノズル
６５ 流量制御器
６７ 開閉バルブ
９０ 制御部
Ｗ ウエハ 4 Processing Vessel 40 Si-Containing Gas Supply Unit 41 Si-Containing Gas Supply Source 42 Si-Containing Gas Pipe 43 Si-Containing Gas Nozzle 44 On-off Valve 45 Flow Controller 46 Storage Unit 47 On-Off Valve 48 Gas Discharge Hole 50 Nitrogen-Containing Gas Supply Unit 51 Nitrogen-Containing Gas supply source 52 Nitrogen-containing gas pipe 53 Nitrogen-containing gas nozzle 55 Flow rate controller 57 Open / close valve 58 Gas discharge hole 60 Purge gas supply unit 61 Purge gas supply source 62 Purge gas pipe 63 Purge gas nozzle 65 Flow rate controller 67 Open / close valve 90 Control unit W Wafer

Claims (12)

原料ガスと反応ガスとを処理容器に収容された基板に対して交互に供給することにより、前記原料ガスと前記反応ガスとの反応により生じる反応生成物の薄膜を前記基板に堆積する成膜方法であって、
貯留部に前記原料ガスを貯留する貯留工程と、
前記貯留部に貯留された前記原料ガスを前記基板に供給し、前記基板に前記原料ガスを吸着させる吸着工程と、
前記原料ガスが吸着した前記基板に前記反応ガスを供給することにより、前記原料ガスと前記反応ガスとを反応させて前記反応生成物を生成する反応工程と、
を有し、
前記貯留工程と、前記吸着工程と、前記反応工程とを複数回繰り返し、複数回繰り返す間に前記貯留工程の条件を少なくとも１回変更する、
成膜方法。 A film forming method for depositing a thin film of a reaction product generated by a reaction between the source gas and the reaction gas on the substrate by alternately supplying the source gas and the reaction gas to the substrate accommodated in the processing container. Because
A storage step of storing the source gas in a storage unit;
An adsorption step of supplying the source gas stored in the storage unit to the substrate and adsorbing the source gas to the substrate;
A reaction step of generating the reaction product by reacting the source gas and the reaction gas by supplying the reaction gas to the substrate on which the source gas is adsorbed;
Have
The storage step, the adsorption step, and the reaction step are repeated a plurality of times, and the conditions of the storage step are changed at least once during a plurality of repetitions.
Film forming method. 前記貯留部は、前記原料ガスの供給源と前記処理容器とを接続する配管に設けられている、
請求項１に記載の成膜方法。 The storage unit is provided in a pipe connecting the source gas supply source and the processing container,
The film forming method according to claim 1. 前記貯留工程は、前記貯留部に前記原料ガスを貯留する条件が互いに異なる第１の貯留工程と第２の貯留工程とを含み、
前記貯留工程と、前記吸着工程と、前記反応工程とを繰り返すごとに、前記第１の貯留工程と前記第２の貯留工程とを交互に繰り返す、
請求項１又は２に記載の成膜方法。 The storage step includes a first storage step and a second storage step in which the conditions for storing the source gas in the storage unit are different from each other,
Each time the storage step, the adsorption step, and the reaction step are repeated, the first storage step and the second storage step are alternately repeated.
The film forming method according to claim 1. 前記第１の貯留工程と前記第２の貯留工程とは、前記貯留部に前記原料ガスを貯留する時間が異なる工程である、
請求項３に記載の成膜方法。 The first storage step and the second storage step are steps in which the time for storing the source gas in the storage unit is different.
The film forming method according to claim 3. 前記第１の貯留工程と前記第２の貯留工程とは、前記原料ガスの供給源から前記貯留部に前記原料ガスを貯留する際の前記原料ガスの流量が異なる工程である、
請求項３に記載の成膜方法。 The first storage step and the second storage step are steps in which the flow rates of the source gas are different when storing the source gas from the source gas supply source to the storage unit.
The film forming method according to claim 3. 前記貯留工程は、前記反応工程が行われている期間に行われる、
請求項１乃至５のいずれか一項に記載の成膜方法。 The storage step is performed during a period in which the reaction step is performed.
The film-forming method as described in any one of Claims 1 thru | or 5. 前記吸着工程と前記反応工程との間に、前記処理容器内にパージガスを供給するパージ工程を有する、
請求項１乃至６のいずれか一項に記載の成膜方法。 A purge step of supplying a purge gas into the processing vessel between the adsorption step and the reaction step;
The film-forming method as described in any one of Claims 1 thru | or 6. 前記吸着工程において、前記基板を回転させた状態で前記基板に前記原料ガスを供給する、
請求項１乃至７のいずれか一項に記載の成膜方法。 In the adsorption step, the source gas is supplied to the substrate while the substrate is rotated.
The film-forming method as described in any one of Claims 1 thru | or 7. 前記吸着工程において、前記原料ガスを前記基板の表面に平行な方向に供給する、
請求項１乃至８のいずれか一項に記載の成膜方法。 In the adsorption step, the source gas is supplied in a direction parallel to the surface of the substrate.
The film-forming method as described in any one of Claims 1 thru | or 8. 前記原料ガスは、シリコン含有ガスである、
請求項１乃至９のいずれか一項に記載の成膜方法。 The source gas is a silicon-containing gas.
The film-forming method as described in any one of Claims 1 thru | or 9. 前記反応ガスは、窒素含有ガスである、
請求項１乃至１０のいずれか一項に記載の成膜方法。 The reaction gas is a nitrogen-containing gas.
The film-forming method as described in any one of Claims 1 thru | or 10. 原料ガスと反応ガスとを基板に対して交互に供給することにより、前記原料ガスと前記反応ガスとの反応により生じる反応生成物の薄膜を前記基板に堆積する成膜システムであって、
貯留部に原料ガスを貯留し、前記貯留部に貯留された前記原料ガスを前記基板に供給する原料ガス供給処理を行う原料ガス供給部と、
前記基板に前記反応ガスを供給する反応ガス供給処理を行う反応ガス供給部と、
前記原料ガス供給処理と、前記反応ガス供給処理とを複数回繰り返し、複数回繰り返す間に前記原料ガス供給処理における前記貯留部に前記原料ガスを貯留する条件を少なくとも１回変更するように、前記原料ガス供給部及び前記反応ガス供給部を制御する制御部と、
を有する、成膜システム。 A film forming system in which a thin film of a reaction product generated by a reaction between the source gas and the reaction gas is deposited on the substrate by alternately supplying a source gas and a reaction gas to the substrate,
A source gas supply unit that stores a source gas in a storage unit and performs a source gas supply process of supplying the source gas stored in the storage unit to the substrate;
A reaction gas supply unit for performing a reaction gas supply process for supplying the reaction gas to the substrate;
The source gas supply process and the reaction gas supply process are repeated a plurality of times, and the conditions for storing the source gas in the storage section in the source gas supply process are changed at least once during the plurality of repetitions. A control unit for controlling the source gas supply unit and the reaction gas supply unit;
A film forming system.
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