JP5342110B2 - Source canister containing precursor and method for filling features using the same - Google Patents

Source canister containing precursor and method for filling features using the same Download PDF

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JP5342110B2
JP5342110B2 JP2006533450A JP2006533450A JP5342110B2 JP 5342110 B2 JP5342110 B2 JP 5342110B2 JP 2006533450 A JP2006533450 A JP 2006533450A JP 2006533450 A JP2006533450 A JP 2006533450A JP 5342110 B2 JP5342110 B2 JP 5342110B2
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tantalum
canister
dimethylamido
substrate
source canister
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JP2007501536A (en
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リン チェン，
ヴィンセント ダブリュー． クー，
フア チャン，
クリストフ マルカダル，
セスハドリ ガングリ，
ジェニー リン，
ディエン − イ− ウー，
アラン オウイ−，
メイ チャン，
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Applied Materials Inc
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Applied Materials Inc
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
    • C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4487—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by using a condenser
    • 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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
    • H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System
    • H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
    • H01L21/28562—Selective deposition
    • 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
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
    • H01L21/76841—Barrier, adhesion or liner layers
    • H01L21/76843—Barrier, adhesion or liner layers formed in openings in a dielectric

Abstract

Embodiments of the present invention are directed to an apparatus for generating a precursor for a semiconductor processing system (320). The apparatus includes a canister (300) having a sidewall (402), a top portion and a bottom portion. The canister (300) defines an interior volume (438) having an upper region (418) and a lower region (434). In one embodiment, the apparatus further includes a heater (430) partially surrounding the canister (300). The heater (430) creates a temperature gradient between the upper region (418) and the lower region (434). Also claimed is a method of forming a barrier layer from purified pentakis (dimethylamido) tantalum, for example a tantalum nitride barrier layer by atomic layer deposition.

Description

発明の背景Background of the Invention

発明の分野
[0001]本発明は、一般的には、半導体基板上にバリヤ層を堆積することに関する。 Field of Invention
[0001] The present invention relates generally to depositing a barrier layer on a semiconductor substrate.

関連技術の記載
[0002]確実にサブミクロン以下の特徴部を製造することは、半導体デバイスの次世代の大面積集積回路（ＶＬＳＩ）や超大面積集積回路（ＵＬＳＩ）の鍵となる技術の一つである。しかしながら、回路の周辺技術が圧縮されるにつれて、ＶＬＳＩやＵＬＳＩ技術における相互接続部の収縮した寸法によって処理能力がさらに要求される。この技術の中心となる多レベル相互接続部には、バイアや他の相互接続部のような高アスペクト比特徴部の正確な処理が必要である。これら相互接続部の確実な形成は、回路密度や個々の基板の質を高めるために、ＶＬＳＩやＵＬＳＩにおける成功と継続した努力が非常に重要である。 Description of related technology
[0002] Certainly producing sub-micron features is one of the key technologies for next-generation large area integrated circuits (VLSI) and ultra large area integrated circuits (ULSI) for semiconductor devices. However, as circuit peripheral technologies are compressed, more processing power is required due to the shrunken dimensions of interconnects in VLSI and ULSI technologies. The multi-level interconnect at the heart of this technology requires the precise processing of high aspect ratio features such as vias and other interconnects. The reliable formation of these interconnects is very important for VLSI and ULSI success and continued efforts to increase circuit density and individual board quality.

[0003]回路密度が増加するにつれて、バイア、コンタクト、他の特徴部、それらの間にある絶縁物質の幅がサブミクロン寸法に縮小し（例えば、約０.２０マイクロメートル未満）、誘電体層の厚さはほぼ一定であり、その結果、特徴部のアスペクト比、即ち、幅で割った高さは増大する。多くの伝統的な堆積プロセスは、アスペクト比が４：１を超える、特に１０：１を超えるサブミクロン構造を満たすことが難しい。それ故、ほぼボイドがなく、アスペクト比が高いシームのないサブミクロン特徴部の形成に多くの継続した努力が向けられている。   [0003] As circuit density increases, the width of vias, contacts, other features, and insulating material between them shrinks to sub-micron dimensions (eg, less than about 0.20 micrometers) and dielectric layers Is substantially constant, and as a result, the aspect ratio of the feature, ie, the height divided by the width, increases. Many traditional deposition processes have difficulty filling submicron structures with aspect ratios greater than 4: 1, especially greater than 10: 1. Therefore, much continued effort is directed to the formation of submicron features that are substantially void free and have high aspect ratio seams.

[0004]現在、銅はアルミニウムより抵抗が小さく（アルミニウムが約３.１μΩ-ｃｍに対して約１.７μΩ-ｃｍ）、電流搬送能が高く、エレクトロマイグレーション耐性が著しく高いことから、銅及びその合金はサブミクロン相互接続部技術の選択金属になってきた。これらの特性は、高レベルの集積度と高デバイス速度で示される更に高い電流密度を支持するのに重要である。更に、銅は良好な導電性であり、高度に純粋な状態で利用できる。   [0004] Currently, copper has a lower resistance than aluminum (aluminum is about 1.7 μΩ-cm compared to about 3.1 μΩ-cm), has a high current carrying capacity, and has a very high resistance to electromigration. Alloys have become the preferred metal for submicron interconnect technology. These properties are important to support the higher current density exhibited by high levels of integration and high device speeds. In addition, copper has good electrical conductivity and is available in a highly pure state.

[0005]銅メタライゼーションは様々な技術により達成され得る。典型的な方法は、一般的には、特徴部上にバリヤ層を堆積する物理的蒸着、バリヤ層上に銅シード層を堆積する物理的蒸着、その後、特徴部を充填する銅シード層上に銅導電材料を電気めっきすることを含んでいる。最後に、堆積された層と誘電体層は、例えば、化学機械的研磨（ＣＭＰ）によって平坦化されて導電性相互接続特徴部を画成する。   [0005] Copper metallization can be accomplished by various techniques. A typical method is generally a physical vapor deposition that deposits a barrier layer on the feature, a physical vapor deposition that deposits a copper seed layer on the barrier layer, and then on the copper seed layer that fills the feature. Including electroplating a copper conductive material. Finally, the deposited layer and the dielectric layer are planarized by, for example, chemical mechanical polishing (CMP) to define conductive interconnect features.

[0006]しかしながら、銅を使用に伴う一つの問題は、シリコン、二酸化シリコン、デバイスの完全さを損なってしまう他の誘電材料に銅が拡散ことである。それ故、コンホーマルなバリヤ層が銅拡散を防止するためにますます重要である。窒化タンタルは下に横たわる層に銅の拡散を防止するバリヤ層として用いられてきた。しかしながら、ペンタキス（ジメチルアミド）タンタル（ＰＤＭＡＴ：Ｔａ[ＮＨ2(ＣＨ3)2]5）のようなバリヤ層堆積に用いられる化学薬品は、半導体デバイスの製造において欠陥を引き起こし、プロセス歩留まりを低下させる不純物を含むものである。それ故、高純度の前駆物質からバリヤ層を堆積する方法が求められている。 [0006] However, one problem with using copper is that it diffuses into silicon, silicon dioxide, and other dielectric materials that compromise device integrity. Therefore, a conformal barrier layer is increasingly important to prevent copper diffusion. Tantalum nitride has been used as a barrier layer to prevent copper diffusion in the underlying layer. However, chemicals used for barrier layer deposition such as pentakis (dimethylamido) tantalum (PDMAT: Ta [NH 2 (CH 3 ) 2 ] 5 ) cause defects in semiconductor device manufacturing and reduce process yield. It contains impurities. Therefore, there is a need for a method of depositing a barrier layer from a high purity precursor.

発明の概要Summary of the Invention

[0007]本発明の実施形態は、半導体処理システムの前駆物質を生成するための装置に関する。装置は、側壁、上部及び底部を有するキャニスタを含む。キャニスタは、上の領域と下の領域を有する内容積を画成する。装置は、更に、キャニスタを取り囲むヒータを含んでいる。ヒータは、上の領域と下の領域との間に温度勾配を生じる。   [0007] Embodiments of the invention relate to an apparatus for producing a precursor for a semiconductor processing system. The apparatus includes a canister having a sidewall, a top and a bottom. The canister defines an internal volume having an upper region and a lower region. The apparatus further includes a heater surrounding the canister. The heater creates a temperature gradient between the upper region and the lower region.

[0008]本発明の上記特徴が得られ、詳細に理解され得るように、上で簡単にまとめられた本発明の更に具体的な説明は添付された図面に示されるその実施形態によってなされる。しかしながら、添付された図面は本発明の典型的な実施形態のみ示され、それ故、本発明の範囲を制限するものとみなすべきでなく、本発明は他の同等に効果的な実施形態を許容することは留意すべきである。   [0008] In order that the above features of the present invention may be obtained and understood in detail, a more particular description of the invention briefly summarized above is made by way of its embodiments that are illustrated in the accompanying drawings. However, the attached drawings show only typical embodiments of the present invention and therefore should not be considered as limiting the scope of the present invention, and the present invention allows other equally effective embodiments. It should be noted that.

好適実施形態の詳細な説明Detailed Description of the Preferred Embodiment

[0020]図１は、基板上に堆積された誘電体層１０２とバリヤ層１０４を有する基板１００の一実施形態の概略断面図である。処理段階によっては、基板１００はシリコン半導体基板又は他の物質層であってもよく、基板上に形成されている。誘電体層１０２は、酸化物、酸化シリコン、炭素シリコン酸化物、フルオロシリコン、多孔質誘電体、又は基板１００の晒された表面部分１０２Ｔに伸びているコンタクトホール又はバイア１０２Ｈを設けるために形成されパターン形成された他の適切な誘電体であってもよい。明瞭にするために、基板１００は膜処理が行われるあらゆる工作物を意味し、基板構造１５０は基板１００と、誘電体層１０２のような基板１００上に形成される他の物質層を示すために用いられる。また、本発明がデュアルダマシンプロセスフローに用いることができることは、当業者によって理解される。バリヤ層１０４は、原子層堆積（ＡＬＤ）により図１Ａの基板構造１５０上に形成される。好ましくは、バリヤ層は窒化タンタル層を含んでいる。   [0020] FIG. 1 is a schematic cross-sectional view of one embodiment of a substrate 100 having a dielectric layer 102 and a barrier layer 104 deposited on the substrate. Depending on the processing stage, the substrate 100 may be a silicon semiconductor substrate or other material layer and is formed on the substrate. Dielectric layer 102 is formed to provide an oxide, silicon oxide, carbon silicon oxide, fluorosilicon, porous dielectric, or contact hole or via 102H extending to the exposed surface portion 102T of substrate 100. Other suitable patterned dielectrics may be used. For the sake of clarity, the substrate 100 refers to any workpiece on which film processing is performed, and the substrate structure 150 is intended to show the substrate 100 and other material layers formed on the substrate 100, such as the dielectric layer 102. Used for. It will also be appreciated by those skilled in the art that the present invention can be used in dual damascene process flows. The barrier layer 104 is formed on the substrate structure 150 of FIG. 1A by atomic layer deposition (ALD). Preferably, the barrier layer includes a tantalum nitride layer.

[0021]一態様においては、窒化タンタルバリヤ層の原子層堆積は、タンタル含有化合物と窒素含有化合物をプロセスチャンバに順次供給することを含んでいる。タンタル含有化合物と窒素含有化合物を連続して供給することにより、基板構造１５０上にタンタル含有化合物の単層と窒素含有化合物の単層の交互化学吸着を得ることができる。   [0021] In one aspect, atomic layer deposition of a tantalum nitride barrier layer includes sequentially supplying a tantalum-containing compound and a nitrogen-containing compound to the process chamber. By continuously supplying the tantalum-containing compound and the nitrogen-containing compound, alternating chemisorption of a single layer of the tantalum-containing compound and a single layer of the nitrogen-containing compound can be obtained on the substrate structure 150.

[0022]図２Ａ-図２Ｃは、集積回路製造の段階、更に詳しくはバリヤ層形成の段階において基板２００の例示的な部分にタンタル含有化合物と窒素含有化合物の単層の交互化学吸着を示す一実施形態である。図２Ａにおいては、タンタル含有化合物の単層は、プロセスチャンバにタンタル含有化合物２０５のパルスを導入することにより基板２００上に化学吸着される。   [0022] FIGS. 2A-2C illustrate an alternate chemisorption of monolayers of a tantalum-containing compound and a nitrogen-containing compound on an exemplary portion of the substrate 200 during integrated circuit fabrication, and more particularly during barrier layer formation. It is an embodiment. In FIG. 2A, a monolayer of tantalum-containing compound is chemisorbed onto substrate 200 by introducing a pulse of tantalum-containing compound 205 into the process chamber.

[0023]タンタル含有化合物２０５は、典型的には、１以上の化学種２１５を有するタンタル原子２１０を含んでいる。一実施形態においては、タンタル含有化合物は、ペンタジメチルアミノ-タンタル（ＰＤＭＡＴ：Ｔａ(ＮＭｅ2)5）である。ＰＤＭＡＴは多くの理由で有利に用いることができる。ＰＤＭＡＴは比較的に安定である。更に、ＰＤＭＡＴは分配を容易にする十分な蒸気圧を有する。特に、ＰＤＭＡＴは低いハライド含有量で製造することができる。ＰＤＭＡＴのハライド含有量は、１００ｐｐｍ未満のハライド含有量で製造すべきである。理論で縛られないならば、バリヤ層に取り込まれるハロゲン（例えば、塩素）はその上に堆積される銅層に結合することができることから、低ハライド含有量を有する有機金属前駆物質が有益であると考えられる。 [0023] The tantalum-containing compound 205 typically includes a tantalum atom 210 having one or more chemical species 215. In one embodiment, the tantalum-containing compound is pentadimethylamino-tantalum (PDMAT: Ta (NMe 2 ) 5 ). PDMAT can be used advantageously for a number of reasons. PDMAT is relatively stable. In addition, PDMAT has sufficient vapor pressure to facilitate distribution. In particular, PDMAT can be produced with a low halide content. The halide content of PDMAT should be produced with a halide content of less than 100 ppm. If not bound by theory, organometallic precursors having a low halide content are beneficial because the halogen (eg, chlorine) incorporated into the barrier layer can bind to the copper layer deposited thereon. it is conceivable that.

[0024]製造中ＰＤＭＡＴの熱分解は、続いて窒化タンタルバリヤ層を形成するために用いられるＰＤＭＡＴ生成物中に不純物を生じることがある。不純物は、ＣＨ3ＮＴａ(Ｎ(ＣＨ3)2)3及び((ＣＨ3)2Ｎ)3Ｔａ(ＮＣＨ2ＣＨ3）のような化合物を含むことができる。更に、水分との反応により、ＰＤＭＡＴ製造中にタンタルオキソアミド化合物が生成することがある。好ましくは、タンタルオキソアミド化合物は昇華によりＰＤＭＡＴから除去される。例えば、タンタルオキソアミド化合物はバブラーにおいて除去される。ＰＤＭＡＴ生成物は約５ｐｐｍ未満の塩素を有することが好ましい。更に、リチウム、鉄、フッ素、臭素、ヨウ素のレベルは最小限にすべきである。更に好ましくは、不純物の全レベルは約５ｐｐｍ未満である。 [0024] Thermal decomposition of PDMAT during manufacture may result in impurities in the PDMAT product that is subsequently used to form a tantalum nitride barrier layer. Impurities can include compounds such as CH 3 NTa (N (CH 3 ) 2 ) 3 and ((CH 3 ) 2 N) 3 Ta (NCH 2 CH 3 ). Furthermore, reaction with moisture may produce tantalum oxoamide compounds during PDMAT production. Preferably, the tantalum oxoamide compound is removed from PDMAT by sublimation. For example, tantalum oxoamide compounds are removed in a bubbler. The PDMAT product preferably has less than about 5 ppm chlorine. Furthermore, the levels of lithium, iron, fluorine, bromine and iodine should be minimized. More preferably, the total level of impurities is less than about 5 ppm.

[0025]タンタル含有化合物はガスとして供給されるか、又はキャリアガスによって供給することができる。用いることができるキャリアガスの例は、ヘリウム（Ｈｅ）、アルゴン（Ａｒ）、窒素（Ｎ2）、水素（Ｈ2）を含むが、これらに限定されない。 [0025] The tantalum-containing compound can be supplied as a gas or can be supplied by a carrier gas. Examples of carrier gases that can be used include, but are not limited to, helium (He), argon (Ar), nitrogen (N 2 ), hydrogen (H 2 ).

[0026]タンタル含有化合物の単層が基板２００に化学吸着された後、過剰なタンタル含有化合物はチャンバへパージガスのパルスを導入することによりプロセスチャンバガスから除去される。用いることができるキャリアガスの例は、ヘリウム（Ｈｅ）、アルゴン（Ａｒ）、窒素（Ｎ2）、水素（Ｈ2）、他のガスを含むが、それらに限定されない。 [0026] After the monolayer of tantalum-containing compound is chemisorbed to substrate 200, excess tantalum-containing compound is removed from the process chamber gas by introducing a pulse of purge gas into the chamber. Examples of carrier gases that can be used include, but are not limited to, helium (He), argon (Ar), nitrogen (N 2 ), hydrogen (H 2 ), other gases.

[0027]図２Ｂを参照すると、プロセスチャンバがパージされた後、窒素含有化合物２２５のパルスがプロセスチャンバに導入される。窒素含有化合物２２５は単独で供給することができ、キャリアガスによって供給することもできる。窒素含有化合物２２５は、１つ以上の反応化学種２３５と窒素原子２３０を含むことができる。窒素含有化合物は、好ましくはアンモニアガス（ＮＨ3）を含んでいる。用いることができる他の窒素含有化合物は、ｘとｙが整数であるＮxＨy（例えば、ヒドラジン（Ｎ2Ｈ4））、ジメチルヒドラジン((ＣＨ3)2Ｎ2Ｈ2）、ｔ-ブチルヒドラジン(Ｃ4Ｈ9Ｎ2Ｈ3），フェニルヒドラジン（Ｃ6Ｈ5Ｎ2Ｈ3）、他のヒドラジン誘導体、窒素プラズマ源（例えばＮ2、Ｎ2/Ｈ2、ＮＨ3又はＮ2Ｈ4プラズマ）、２,２’-アゾイソブタン((ＣＨ3)6Ｃ2Ｎ2）、エチルアジド（Ｃ2Ｈ5Ｎ3）、及び他の適切なガスを含むことができる。キャリアガスは、必要ならば窒素含有化合物を分配するために用いることができる。 [0027] Referring to FIG. 2B, after the process chamber is purged, a pulse of nitrogen-containing compound 225 is introduced into the process chamber. The nitrogen-containing compound 225 can be supplied alone or can be supplied by a carrier gas. Nitrogen-containing compound 225 can include one or more reactive species 235 and nitrogen atom 230. The nitrogen-containing compound preferably contains ammonia gas (NH 3 ). Other nitrogen-containing compounds that can be used include N x H y (eg, hydrazine (N 2 H 4 )), dimethyl hydrazine ((CH 3 ) 2 N 2 H 2 ), t − where x and y are integers. Butyl hydrazine (C 4 H 9 N 2 H 3 ), phenyl hydrazine (C 6 H 5 N 2 H 3 ), other hydrazine derivatives, nitrogen plasma sources (eg N 2 , N 2 / H 2 , NH 3 or N 2 H 4 plasma), 2,2′-azoisobutane ((CH 3 ) 6 C 2 N 2 ), ethyl azide (C 2 H 5 N 3 ), and other suitable gases. The carrier gas can be used to distribute the nitrogen-containing compound if necessary.

[0028]窒素含有化合物２２５の単層は、タンタル含有化合物２０５の単層に化学吸着されてもよい。原子層堆積（ＡＬＤ）の間の表面上における前駆物質の組成と構造は正確には不明である。理論で縛られないなら、窒素含有化合物２２５の化学吸着した単層は、タンタル含有化合物２０５の単層と反応して窒化タンタル層２０９を形成する。反応化学種２１５、２３５は、真空システムにより基板表面から輸送される副生成物２４０を形成する。   [0028] The monolayer of nitrogen-containing compound 225 may be chemisorbed to the monolayer of tantalum-containing compound 205. The composition and structure of the precursor on the surface during atomic layer deposition (ALD) is not exactly known. If not bound by theory, the chemisorbed monolayer of nitrogen-containing compound 225 reacts with the monolayer of tantalum-containing compound 205 to form tantalum nitride layer 209. The reactive species 215, 235 form a byproduct 240 that is transported from the substrate surface by the vacuum system.

[0029]窒素含有化合物２２５の単層がタンタル含有化合物の単層上に化学吸着されると、あらゆる過剰な窒素含有化合物が、チャンバにパージガスの他のパルスを導入することによりプロセスチャンバから除去される。その後、図２Ｃに示されるように、タンタル含有化合物と窒素含有化合物の単層の交互化学吸着の窒化タンタル層堆積シーケンスを繰り返すことができる。   [0029] Once the monolayer of nitrogen-containing compound 225 is chemisorbed onto the monolayer of tantalum-containing compound, any excess nitrogen-containing compound is removed from the process chamber by introducing another pulse of purge gas into the chamber. The The tantalum nitride layer deposition sequence of alternating chemisorption of a single layer of tantalum-containing compound and nitrogen-containing compound can then be repeated, as shown in FIG. 2C.

[0030]図２Ａ-図２Ｃにおいては、窒化タンタル層形成は、基板上のタンタル含有化合物の単層の化学吸着から出発して、続いて窒素含有化合物の単層の化学吸着が示されている。或いは、窒化タンタル層形成は、基板上の窒素含有化合物の単層の化学吸着から開始することができ、続いてタンタル含有化合物の単層が化学吸着される。更に、代替実施形態においては、反応ガスのパルス間だけのポンプ排気は反応ガスの混合を防止するために用いることができる。   [0030] In FIGS. 2A-2C, tantalum nitride layer formation is shown starting with a monolayer chemisorption of a tantalum-containing compound on a substrate followed by a monolayer chemisorption of a nitrogen-containing compound. . Alternatively, tantalum nitride layer formation can begin with chemisorption of a nitrogen-containing compound monolayer on the substrate followed by chemisorption of the tantalum-containing compound monolayer. Further, in an alternative embodiment, pumping only during the reaction gas pulses may be used to prevent reaction gas mixing.

[0031]タンタル含有化合物、窒素含有化合物、パージガスの各パルスの持続時間は可変であり、用いられる堆積チャンバとそれに結合される真空システムのだけでなく堆積チャンバに必要とされる容積能力に左右される。例えば、（１）低いガスのチャンバ圧より長いパルス時間を必要とし；（２）低いガス流量は、チャンバ圧が上昇し安定化するのに長い時間を必要とし、長いパルス時間を必要とする；（３）大容積チャンバが充填するのに長い時間かかり、チャンバ圧が安定化するのに長くかかるので、長いパルス時間が必要である。同様に、各パルス間の時間も可変であり、プロセスチャンバの容積能力とそれに結合される真空システムに左右される。通常、タンタル含有化合物又は窒素含有化合物のパルスの持続時間は、化合物の単層の化学吸着に十分に長くすべきである。通常、パージガスのパルス時間は、反応副生成物及び/又はプロセスチャンバに残留するあらゆる残留物質を除去するために十分に長くすべきである。   [0031] The duration of each pulse of tantalum-containing compound, nitrogen-containing compound, and purge gas is variable and depends on the volumetric capacity required of the deposition chamber as well as the deposition chamber used and the vacuum system coupled to it. The For example, (1) a longer pulse time is required than the low gas chamber pressure; (2) a low gas flow rate requires a long time and a long pulse time for the chamber pressure to rise and stabilize; (3) It takes a long time to fill the large volume chamber and it takes a long time for the chamber pressure to stabilize, so a long pulse time is required. Similarly, the time between each pulse is variable and depends on the volume capacity of the process chamber and the vacuum system coupled to it. In general, the duration of a pulse of a tantalum-containing compound or a nitrogen-containing compound should be long enough for chemisorption of a single layer of the compound. Typically, the purge gas pulse time should be sufficiently long to remove reaction by-products and / or any residual material remaining in the process chamber.

[0032]通常、タンタル含有化合物の１.０秒以下のパルス時間、窒素含有化合物の約１.０秒以下のパルス時間は、基板上の交互単層を化学吸着させるために典型的には十分である。パージガスの約１.０秒以下のパルス時間は、プロセスチャンバに残存する反応副生成物とあらゆる残留物質を除去するのに典型的には十分である。もちろん、長いパルス時間がタンタル含有化合物と窒素含有化合物の化学吸着を確実にするとともに反応副生成物の除去を確実にするために用いることができる。   [0032] Typically, pulse times of 1.0 seconds or less for tantalum-containing compounds and pulse times of about 1.0 seconds or less for nitrogen-containing compounds are typically sufficient to chemisorb alternating monolayers on a substrate. It is. A pulse time of about 1.0 second or less of the purge gas is typically sufficient to remove any reaction byproducts and any remaining material remaining in the process chamber. Of course, long pulse times can be used to ensure chemisorption of tantalum-containing and nitrogen-containing compounds and to ensure removal of reaction byproducts.

[0033]原子層堆積の間、基板は選択されたタンタル含有化合物の熱分解温度より大体低く維持することができる。本明細書に確認されたタンタル含有化合物において用いられる典型的なヒータ温度範囲は、約１００ｔｏｒｒ未満のチャンバ圧、好ましくは５０ｔｏｒｒ未満で約２０℃〜約５００℃である。タンタル含有ガスがＰＤＭＡＴであるとき、ヒータ温度は、好ましくは約１７５℃〜約２５０℃、更に好ましくは約１００℃〜約３００℃である。他の実施形態においては、他の温度を用いることができることを理解すべきである。例えば、熱分解温度より高い温度を用いることができる。しかしながら、温度は、５０％を超える堆積活性が化学吸着プロセスによるように選択すべきである。他の例においては、成長方式が原子層堆積成長方式と類似するように各前駆物質堆積中の熱分解量が制限される熱分解温度より高い温度を用いることができる。   [0033] During atomic layer deposition, the substrate can be maintained approximately below the thermal decomposition temperature of the selected tantalum-containing compound. A typical heater temperature range used in the tantalum-containing compounds identified herein is a chamber pressure of less than about 100 torr, preferably from about 20 ° C. to about 500 ° C. at less than 50 torr. When the tantalum-containing gas is PDMAT, the heater temperature is preferably about 175 ° C to about 250 ° C, more preferably about 100 ° C to about 300 ° C. It should be understood that other temperatures can be used in other embodiments. For example, a temperature higher than the thermal decomposition temperature can be used. However, the temperature should be chosen such that a deposition activity of more than 50% is due to the chemisorption process. In another example, a temperature higher than the pyrolysis temperature at which the amount of pyrolysis during each precursor deposition is limited can be used so that the growth scheme is similar to the atomic layer deposition growth scheme.

[0034]プロセスチャンバにおいて原子層堆積によって窒化タンタル層を堆積する一例示的なプロセスは、順次、ペンタジメチルアミノタンタル（ＰＤＭＡＴ）を約１００ｓｃｃｍ〜約１０００ｓｃｃｍ、好ましくは約２００ｓｃｃｍ〜約５００ｓｃｃｍの流量で約１.０秒以下の時間、供給するステップ、アンモニアを約１００ｓｃｃｍ〜約１０００ｓｃｃｍ、好ましくは約２００ｓｃｃｍ〜約５００ｓｃｃｍの流量で約１.０秒以下の時間、供給するステップ、パージガスを約１００ｓｃｃｍ〜約１０００ｓｃｃｍ、好ましくは約２００ｓｃｃｍ〜約５００ｓｃｃｍの流量で約１.０秒以下の時間、供給するステップを含んでいる。ヒータ温度は、好ましくは約１.０〜約５.０ｔｏｒｒのチャンバ圧で約１００℃〜約３００℃で維持される。交互のシーケンスは、所望の厚さが達成されるまで繰り返すことができる。   [0034] One exemplary process for depositing a tantalum nitride layer by atomic layer deposition in a process chamber is followed by about pentadimethylamino tantalum (PDMAT) at a flow rate of about 100 seem to about 1000 seem, preferably about 200 seem to about 500 seem. Supplying for 1.0 second or less, supplying ammonia at a flow rate of about 100 sccm to about 1000 sccm, preferably about 200 sccm to about 500 sccm for about 1.0 second or less, purging gas for about 100 sccm to about 1000 sccm And supplying at a flow rate of preferably about 200 seem to about 500 seem for a time of about 1.0 seconds or less. The heater temperature is preferably maintained at about 100 ° C. to about 300 ° C. with a chamber pressure of about 1.0 to about 5.0 torr. The alternating sequence can be repeated until the desired thickness is achieved.

[0035]図３は、本発明の態様に従って原子層堆積により１以上バリヤ層を形成するために用いることができる、処理システム３２０の一例示的実施形態の概略断面図である。もちろん、他の処理システムを用いることもできる。   [0035] FIG. 3 is a schematic cross-sectional view of one exemplary embodiment of a processing system 320 that can be used to form one or more barrier layers by atomic layer deposition according to aspects of the present invention. Of course, other processing systems can be used.

[0036]処理システム３２０は、通常は、ガス分配システム３０４に結合したプ処理チャンバ３０６を含んでいる。処理チャンバ３０６は、例えば、カリフォルニア州サンタクララにあるアプライドマテリアルズ社から入手できる、適切なあらゆるプロセスチャンバであってもよい。例示的なプロセスチャンバは、特に、ＤＰＳＣＥＮＴＵＲＡ(登録商標)エッチングチャンバ、ＰＲＯＤＵＣＥＲ(登録商標)化学気相堆積チャンバ、ＥＮＤＵＲＡ(登録商標)物理気相堆積チャンバを含んでいる。   [0036] The processing system 320 typically includes a processing chamber 306 coupled to a gas distribution system 304. The processing chamber 306 may be any suitable process chamber available, for example, from Applied Materials, Inc., located in Santa Clara, California. Exemplary process chambers include, among other things, the DPSCENTURA® etch chamber, the PRODUCER® chemical vapor deposition chamber, and the ENDURA® physical vapor deposition chamber.

[0037]ガス分配システム３０４は、通常、様々なプロセスガスや不活性ガスが処理チャンバ３０６に分配される際の速度と圧力を制御する。処理チャンバ３０６に分配されるプロセスガスや他のガスの数と種類は、通常、それに結合した処理チャンバ３０６で行われるプロセスに基づいて選択される。簡単のために、単一ガス分配回路が図３に示されるガス分配システム３０４に示されるが、更にガス分配回路を用いることができることは予想される。   [0037] The gas distribution system 304 typically controls the rate and pressure at which various process and inert gases are distributed to the processing chamber 306. The number and type of process gases and other gases dispensed into the processing chamber 306 are typically selected based on the processes performed in the processing chamber 306 coupled thereto. For simplicity, a single gas distribution circuit is shown in the gas distribution system 304 shown in FIG. 3, but it is anticipated that further gas distribution circuits can be used.

[0038]ガス分配システム３０４は、通常は、キャリアガス源３０２とプロセスチャンバ３０６間に結合される。キャリアガス源３０２は局部容器又は遠隔容器又は設備全体にキャリアガスを供給する集中設備供給源であってもよい。キャリアガス源３０２は、典型的には、キャリアガス、例えば、アルゴン、窒素、ヘリウム又は他の不活性又は非反応性ガスを供給する。   [0038] A gas distribution system 304 is typically coupled between the carrier gas source 302 and the process chamber 306. The carrier gas source 302 may be a local facility or a remote facility or a central facility supply that supplies carrier gas to the entire facility. The carrier gas source 302 typically supplies a carrier gas, such as argon, nitrogen, helium or other inert or non-reactive gas.

[0039]ガス分配システム３０４は、典型的には、キャリアガス源３０２とプロセスガスソースキャニスタ３００間に結合したフローコントローラ３１０を含んでいる。フローコントローラ３１０は、比例バルブ、調節バルブ、ニードルバルブ、レギュレータ、マスフローコントローラ等であってもい。用いることができる一フローコントローラ３１０は、カリフォルニア州モントレーにあるＳｉｅｒｒａＩｎｓｔｒｕｍｅｎｔｓ社から入手できる。   [0039] The gas distribution system 304 typically includes a flow controller 310 coupled between the carrier gas source 302 and the process gas source canister 300. The flow controller 310 may be a proportional valve, a regulating valve, a needle valve, a regulator, a mass flow controller, or the like. One flow controller 310 that can be used is available from Sierra Instruments, Inc., located in Monterey, California.

[0040]ソースキャニスタ３００は、典型的には、第一、第二バルブ３１２、３１４間に結合し、配置される。一実施形態においては、第一、第二バルブ３１２、３１４はソースキャニスタ３００に結合され、ガス分配システム３０４からソースキャニスタ３００と共にバルブ３１２、３１４を容易に取り外せるように、切断取り付け具（図示せず）で取り付けられている。第三バルブ３１６は、ガス分配システム３０４からソースキャニスタ３００を取り外した後、処理チャンバ３０６への汚染物質の導入を防止するために第二バルブ３１４と処理チャンバ３０６間に配置される。   [0040] The source canister 300 is typically coupled and disposed between the first and second valves 312,314. In one embodiment, the first and second valves 312, 314 are coupled to the source canister 300 and a cutting fixture (not shown) so that the valves 312, 314 can be easily removed from the gas distribution system 304 along with the source canister 300. ). The third valve 316 is disposed between the second valve 314 and the processing chamber 306 to prevent introduction of contaminants into the processing chamber 306 after removing the source canister 300 from the gas distribution system 304.

[0041]図４Ａと図４Ｂは、ソースキャニスタ３００の一実施形態を示す断面図である。ソースキャニスタ３００は、通常は、プロセス（又は他の）ガスが昇華又は気化プロセスによって生成することができる前駆物質４１４を保持するように適合されているハウジング４２０を有するアンプル又は他の密封容器を含んでいる。昇華プロセスによってソースキャニスタ３００にプロセスガスを生成することができるある固体前駆物質４１４は、特に、二フッ化キセノン、ニッケルカルボニル、タングステンヘキサカルボニル、ペンタキス(ジメチルアミノ)タンタル（ＰＤＭＡＴ）を含んでいる。気化プロセスによってソースキャニスタ３００にプロセスガスを生成することができるある液体前駆物質４１４は、特に、テトラキス(ジメチルアミノ)チタン（ＴＤＭＡＴ）、ｔｅｒｔ-ブチルイミノトリス(ジエチルアミノ)タンタル（ＴＢＴＤＥＴ）、ペンタキス(エチルメチルアミノ)タンタル（ＰＤＭＡＴ）を含んでいる。ハウジング４２０は、前駆物質４１４やそれから生成されたガスに実質的に不活性な物質から通常は製造されるので、物質の構成は生成されるガスに基づいて変化し得る。   [0041] FIGS. 4A and 4B are cross-sectional views illustrating one embodiment of a source canister 300. FIG. The source canister 300 typically includes an ampoule or other sealed container having a housing 420 that is adapted to hold a precursor 414 from which process (or other) gas can be generated by a sublimation or vaporization process. It is out. Some solid precursors 414 that can generate process gases in the source canister 300 by a sublimation process include, among others, xenon difluoride, nickel carbonyl, tungsten hexacarbonyl, pentakis (dimethylamino) tantalum (PDMAT). Some liquid precursors 414 that can generate a process gas in the source canister 300 by a vaporization process include tetrakis (dimethylamino) titanium (TDMAT), tert-butyliminotris (diethylamino) tantalum (TBTDET), pentakis (ethyl), among others. Methylamino) tantalum (PDMAT). Since the housing 420 is typically manufactured from a material that is substantially inert to the precursor 414 and the gas produced therefrom, the composition of the material can vary based on the gas produced.

[0042]ハウジング４２０は、多くの幾何学的形を有することができる。図４Ａと図４Ｂに示される実施形態においては、ハウジング４２０は、円柱状側壁４０２とリッド４０４により密封された底面４３２を含んでいる。リッド４０４は、溶接、結合、接着、又は他の漏れない方法で側壁４０２に結合することができる。或いは、側壁４０２とリッド４０４間の連結は、シール、ｏ-リング、ガスケット等を有し、ソースキャニスタ３００からの漏れを防止するために配置されている。或いは、側壁４０２は、例えば、中空平方チューブの他の中空幾何学的形を含むことができる。   [0042] The housing 420 can have many geometric shapes. In the embodiment shown in FIGS. 4A and 4B, the housing 420 includes a cylindrical side wall 402 and a bottom surface 432 sealed by a lid 404. The lid 404 can be coupled to the sidewall 402 by welding, bonding, gluing, or other leak-proof method. Alternatively, the connection between the side wall 402 and the lid 404 includes a seal, o-ring, gasket, etc. and is arranged to prevent leakage from the source canister 300. Alternatively, the side wall 402 may include other hollow geometric shapes, for example, a hollow square tube.

[0043]流入ポート４０６と流出ポート４０８は、ガスフローをソースキャニスタ３００の内外に流すことを可能にするソースキャニスタによって形成されている。ポート４０６、４０８は、ソースキャニスタ３００のリッド４０４及び/又は側壁４０２によって形成することができる。ポート４０６、４０８は、ガス分配システム３０４からソースキャニスタ３００の取り外し中に、ソースキャニスタ３００の内部を周囲環境から分離することを可能にするように通常は密封可能である。一実施形態においては、バルブ３１２、３１４は、前駆物質４１４の再充填又はソースキャニスタ３００の取替えるために、ガス分配システム３０４（図３に示される）から取り外されるとき、ソースキャニスタ３００からの漏れを防止するためにポート４０６、４０８と密封して結合される。一対の切断取り付け具４３６Ａ、４３６Ｂは、ガス分配システム３０４に、また、ガス分配システムからソースキャニスタ３００の取り外しや取替えを容易にするために、バルブ３１２と３１４に結合することができる。バルブ３１２、３１４は、典型的には、充填、輸送、又はガス分配システム３０４への結合中にソースキャニスタ３００からの潜在的な漏れを最少にしつつ、ソースキャニスタ３００が効率的に装填されたシステムから取り外され再循環させることができるボールバルブ又は確実に密封されるバルブである。或いは、ソースキャニスタ３００は、ソースキャニスタ３００のリッド４０４に配置されるＶＣＲ取付け具で小チューブのような再充填ポート（図示せず）によって再充填され得る。   [0043] The inflow port 406 and the outflow port 408 are formed by a source canister that allows gas flow to flow in and out of the source canister 300. Ports 406, 408 can be formed by lid 404 and / or sidewall 402 of source canister 300. Ports 406, 408 are typically sealable to allow the interior of source canister 300 to be isolated from the ambient environment during removal of source canister 300 from gas distribution system 304. In one embodiment, valves 312, 314 may leak from source canister 300 when removed from gas distribution system 304 (shown in FIG. 3) to refill precursor 414 or replace source canister 300. In order to prevent, it is hermetically coupled with the ports 406, 408. A pair of cutting fixtures 436A, 436B can be coupled to the gas distribution system 304 and to the valves 312 and 314 to facilitate removal and replacement of the source canister 300 from the gas distribution system. Valves 312, 314 are typically systems that are efficiently loaded with source canister 300 while minimizing potential leakage from source canister 300 during filling, transport, or coupling to gas distribution system 304. A ball valve that can be removed from and recirculated or a valve that is securely sealed. Alternatively, the source canister 300 can be refilled by a refill port (not shown) such as a small tube with a VCR fitting located on the lid 404 of the source canister 300.

[0044]ソースキャニスタ３００は、上部領域４１８と下部領域４３４を有する内容積４３８を有する。ソースキャニスタ３００の下部領域４３４は、前駆物質４１４で少なくとも部分的に充填される。或いは、液体４１６はスラリー４１２を形成するために固体前駆物質４１４に加えることができる。前駆物質４１４、液体４１６、又は前もって混合したスラリー４１２は、リッド４０４を取り外すことにより、又はポート４０６、４０８の１つによってソースキャニスタ内に導入することができる。液体４１６は前駆物質４１４と非反応せいであり、前駆物質４１４は液体４１６内で不溶解であるように、液体４１６が前駆物質４１４と比較して無視できるほどの蒸気圧を有するように、液体４１６に、例えば、タングステンヘキサカルボニルの固体前駆物質４１４の蒸気圧の比率が１０3を超えるように選ばれる。 [0044] The source canister 300 has an internal volume 438 having an upper region 418 and a lower region 434. The lower region 434 of the source canister 300 is at least partially filled with the precursor 414. Alternatively, liquid 416 can be added to solid precursor 414 to form slurry 412. Precursor 414, liquid 416, or premixed slurry 412 can be introduced into the source canister by removing lid 404 or by one of ports 406, 408. The liquid 416 is non-reactive with the precursor 414 and the liquid 416 has a negligible vapor pressure compared to the precursor 414 so that the precursor 414 is insoluble in the liquid 416. For example, 416 is selected such that the vapor pressure ratio of tungsten hexacarbonyl solid precursor 414 exceeds 10 3 .

[0045]液体４１６と混合した前駆物質４１４は、スラリー４１２中の液体４１６に懸濁した前駆物質４１４を維持するように時々攪拌することができる。一実施形態においては、前駆物質４１４と液体４１６は磁気スターラー４４０によって攪拌される。磁気スターラー４４０は、ソースキャニスタ３００の底面４３２の下に配置される磁気モータ４４２とソースキャニスタ３００の下部領域４３４に配置された磁気ピル４４４を含んでいる。磁気モータ４４２はソースキャニスタ３００内の磁気ピル４４４を回転させるように作動させ、それによりスラリー４１２を混合する。磁気ピル４４４は、前駆物質４１４、液体４１６、又はソースキャニスタ３００と非反応性である物質の外部コーティングを有するべきである。適切な磁気ミキサは市販されている。適切な磁気ミキサの一例は、ノースカリフォルニア州のウィルミントンのＩＫＡ(登録商標) Ｗｏｒｋｓから入手できるＩＫＡＭＡＧ(登録商標) ＲＥＯである。或いは、スラリー４１２は、ミキサ、バブラー等の他の手段で攪拌することができる。   [0045] The precursor 414 mixed with the liquid 416 can be occasionally agitated to maintain the precursor 414 suspended in the liquid 416 in the slurry 412. In one embodiment, precursor 414 and liquid 416 are agitated by magnetic stirrer 440. The magnetic stirrer 440 includes a magnetic motor 442 disposed below the bottom surface 432 of the source canister 300 and a magnetic pill 444 disposed in the lower region 434 of the source canister 300. The magnetic motor 442 operates to rotate the magnetic pill 444 in the source canister 300, thereby mixing the slurry 412. The magnetic pill 444 should have an outer coating of material that is non-reactive with the precursor 414, liquid 416, or source canister 300. Suitable magnetic mixers are commercially available. An example of a suitable magnetic mixer is IKAMAG® REO available from IKA® Works, Wilmington, North California. Alternatively, the slurry 412 can be stirred by other means such as a mixer or a bubbler.

[0046]液体４１６の攪拌によって、液体４１６の小滴がキャリアガスに移動し処理チャンバ３０６に向かって送られるように誘導することができる。このような液体４１６の小滴が処理チャンバ３０６に到達することを防止するために、オイルトラップ４５０がソースキャニスタ３００の流出ポート４０８に任意に懸濁することができる。オイルトラップ４５０は、オイルトラップ本体４５２の中央線４５６をこえて伸び、ソースキャニスタ３００へ少なくともわずかに下向きに傾いている複数のすきまのあるバッフル４５４を含有する本体４５２を含んでいる。バッフル４５４によって、プロセスチャンバ３０６に向かって流れるガスが進みバッフル４５４の周りの捻じれた経路に流れるる。バッフル４５４の表面積によって、ガスに移動することができるオイル小滴が付着する流れているガスにさらされた大表面積が得られる。バッフル４５４の下向きの角度は、全てのオイルがソースキャニスタ３００に下向きと後ろに流れるオイルトラップに蓄積させることができる。   [0046] Agitation of the liquid 416 may induce a droplet of the liquid 416 to move to the carrier gas and be sent toward the processing chamber 306. In order to prevent such droplets of liquid 416 from reaching the processing chamber 306, the oil trap 450 can optionally be suspended in the outlet port 408 of the source canister 300. The oil trap 450 includes a body 452 that includes a plurality of clearance baffles 454 that extend beyond the center line 456 of the oil trap body 452 and that are inclined at least slightly downwardly toward the source canister 300. The baffle 454 advances the gas flowing toward the process chamber 306 and flows in a twisted path around the baffle 454. The surface area of the baffle 454 provides a large surface area exposed to the flowing gas to which oil droplets that can move into the gas adhere. The downward angle of the baffle 454 allows all oil to accumulate in an oil trap that flows downward and back into the source canister 300.

[0047]ソースキャニスタ３００は、ソースキャニスタ３００の上部領域４１８内に配置された少なくとも１つのバッフル４１０を含んでいる。バッフル４１０は流入ポート４０６と流出ポート４０８間に配置され、伸張した平均流路がつくられ、それにより流入ポート４０６から流出ポート４０８へのキャリアガスの直接（即ち、直線）のフローが防止される。このことは、ソースキャニスタ３００内のキャリアガスの平均滞留時間を増加させるとともにキャリアガスにより送られた昇華又は気化された前駆物質ガスの量を増加させる効果を有する。更に、バッフル４１０は、ソースキャニスタ３００に配置された前駆物質４１４の晒された表面全体にキャリアガスを送り、前駆物質４１４の再現性のあるガス生成特性と効率的な消費を確実にする。   [0047] The source canister 300 includes at least one baffle 410 disposed in the upper region 418 of the source canister 300. The baffle 410 is disposed between the inflow port 406 and the outflow port 408 to create an elongated average flow path, thereby preventing direct (ie, straight) flow of carrier gas from the inflow port 406 to the outflow port 408. . This has the effect of increasing the average residence time of the carrier gas in the source canister 300 and increasing the amount of sublimated or vaporized precursor gas sent by the carrier gas. In addition, the baffle 410 delivers a carrier gas across the exposed surface of the precursor 414 located in the source canister 300 to ensure reproducible gas generation characteristics and efficient consumption of the precursor 414.

[0048]バッフル４１０の数、間隔、形は、前駆物質ガスの最適生成のためにソースキャニスタ３００が合うように選択することができる。例えば、多くのバッフル４１０が前駆物質４１４に更に高いキャリアガス速度を与えるように選択することができ又はバッフル４１０の形が更に効率的な前駆物質の使用のために前駆物質４１４の消費を制御するよう構成することができる。   [0048] The number, spacing, and shape of the baffles 410 can be selected to suit the source canister 300 for optimal production of precursor gases. For example, many baffles 410 can be selected to give the precursor 414 a higher carrier gas velocity, or the shape of the baffle 410 controls the consumption of the precursor 414 for more efficient precursor use. It can be configured as follows.

[0049]バッフル４１０は、側壁４０２又はリッド４０４に結合することができ、又はバッフル４１０はソースキャニスタ３００内に適合するように設計された前もって製造された挿入物であってもよい。一実施形態においては、ソースキャニスタ３００内に配置されたバッフル４１０は、側壁４０２と同様の物質で製造された五枚の矩形プレートを含んでいる。図４Ｂを参照すると、バッフル４１０は相互に平行な側壁４０２に溶接されるか或いは固定される。バッフル４１０はすきまがあり、交互方法でソースキャニスタの対向する側壁に固定され、曲った伸長平均流路が作られる。更に、バッフル４１０は、側壁４０２上に載置されたとき、リッド４０４上の流入ポート４０６と流出ポート４０８との間に置かれ、バッフル４１０とリッド４０４との間に空間が無いように配置されている。バッフル４１０は、更に、ソースキャニスタ３００の下部領域４３４に少なくとも部分的に伸長しているので、上の領域に流れ込むキャリアガスの伸長した平均流路を画成する。   [0049] The baffle 410 can be coupled to the sidewall 402 or the lid 404, or the baffle 410 can be a pre-fabricated insert designed to fit within the source canister 300. In one embodiment, the baffle 410 disposed within the source canister 300 includes five rectangular plates made of a material similar to the sidewall 402. Referring to FIG. 4B, the baffle 410 is welded or secured to the side walls 402 that are parallel to each other. The baffle 410 has a gap and is fixed to the opposite side walls of the source canister in an alternating manner, creating a curved elongated average flow path. Further, when the baffle 410 is placed on the side wall 402, the baffle 410 is placed between the inflow port 406 and the outflow port 408 on the lid 404, and there is no space between the baffle 410 and the lid 404. ing. The baffle 410 further extends at least partially into the lower region 434 of the source canister 300 and thus defines an extended average flow path for carrier gas flowing into the upper region.

[0050]任意に、注入チューブ４２２をソースキャニスタ３００の内部領域４３８に配置することができる。チューブ４２２はソースキャニスタ３００の流入ポート４０６に第一端４２４によって結合され、ソースキャニスタ３００の上部領域４１８内において第二端４２６で終わる。チューブ４２２は、前駆物質４１４又はスラリー４１２に近い位置でソースキャニスタ３００の上部領域４１８にキャリアガスを注入する。   [0050] Optionally, the infusion tube 422 can be placed in the interior region 438 of the source canister 300. Tube 422 is coupled to inflow port 406 of source canister 300 by first end 424 and terminates at second end 426 within upper region 418 of source canister 300. The tube 422 injects carrier gas into the upper region 418 of the source canister 300 at a location near the precursor 414 or slurry 412.

[0051]前駆物質４１４は、前もって設定された温度と圧力で前駆ガスを生成する。前駆物質４１４から昇華又は気化されたガスはソースキャニスタ３００の上の領域に蓄積され、流入ポート４０６を通って入り流出ポート４０８を出る不活性のキャリアガスにより押し出され、処理チャンバ３０６に送られる。一実施形態においては、前駆物質４１４は側壁４０２の近くに配置された抵抗ヒータ４３０によって前もって設定された温度に加熱される。或いは、前駆物質４１４は、ソースキャニスタ３００の上部領域４１８又は下部領域４３４に配置されたカートリッジヒータ（図示せず）のような他の手段によって又はキャリアガス流入ポート４０６の上流に配置されたヒータ（図示せず）でキャリアガスを予熱することにより加熱することができる。スラリー４１２全体に均一な熱拡散を最大にするために、液体４１６とバッフル４１０は良好な導体でなければならない。   [0051] The precursor 414 generates a precursor gas at a preset temperature and pressure. Sublimated or vaporized gas from the precursor 414 accumulates in the region above the source canister 300, is pushed out by the inert carrier gas that enters through the inflow port 406 and exits the outflow port 408, and is sent to the processing chamber 306. In one embodiment, the precursor 414 is heated to a preset temperature by a resistance heater 430 positioned near the sidewall 402. Alternatively, the precursor 414 may be heated by other means such as a cartridge heater (not shown) disposed in the upper region 418 or lower region 434 of the source canister 300 or upstream of the carrier gas inlet port 406 ( It is possible to heat the carrier gas by preheating it (not shown). In order to maximize uniform heat diffusion throughout the slurry 412, the liquid 416 and the baffle 410 must be good conductors.

[0052]本発明の更に他の実施形態によれば、窒化アルミニウム又は窒化ホウ素のような熱導電性の高い多数の固体ビーズ又は粒子８１０を、図８に示されるように、液体４１６の代わりに用いることができる。このような固体粒子８１０は、液体４１６よりキャニスタ８００の側壁から前駆物質４１４に更に多くの熱を伝達させるために用いることができる。固体粒子８１０は、前駆物質４１４と非反応性であり、不溶であり、前駆物質４１４と比較して無視できるほどの蒸気圧を有するという点で液体４１６と同じ特性を有する。そういうものとして、固体粒子８１０はキャニスタ８００の側壁からキャニスタ８００の中心部に熱を効率的に伝達するよう構成され、それにより昇華又は気化中に更に多くの前駆物質が用いられる。固体粒子８１０は、また、キャニスタ８００に堆積される前に、汚染物質、水蒸気等を脱ガスし洗浄することができる。   [0052] According to yet another embodiment of the present invention, a large number of highly thermally conductive solid beads or particles 810, such as aluminum nitride or boron nitride, are substituted for liquid 416, as shown in FIG. Can be used. Such solid particles 810 can be used to transfer more heat from the sidewalls of the canister 800 to the precursor 414 than the liquid 416. Solid particles 810 have the same characteristics as liquid 416 in that they are non-reactive with precursor 414, insoluble, and have negligible vapor pressure compared to precursor 414. As such, the solid particles 810 are configured to efficiently transfer heat from the sidewalls of the canister 800 to the center of the canister 800, thereby using more precursors during sublimation or vaporization. The solid particles 810 can also be degassed and cleaned of contaminants, water vapor, etc. before being deposited on the canister 800.

[0053]動作の一例示的方法においては、ソースキャニスタ３００の下部領域４３４は、タングステンヘキサカルボニルと拡散ポンプオイルの混合物で少なくとも部分的に充填されてスラリー４１２を形成する。スラリー４１２は約５Ｔｏｒｒの圧力に保たれ、ソースキャニスタ３００の近くにある抵抗ヒータ４３０によって摂氏約４０度〜摂氏約５０度の範囲の温度に加熱される。アルゴンの形でのキャリアガスは、約４００標準ｃｃ/ｍｉｎの速度で上部領域４１８に流入ポート４０６を通って流れる。アルゴンは、流出ポート４０８によってソースキャニスタ３００を出る前に、バッフル４１０によって捻じれた流路により画成された伸長した平均流路に流れ、有利にはソースキャニスタ３００の上部領域４１８におけるアルゴンの平均滞留時間が長くなる。ソースキャニスタ３００内の長い滞留時間によって、有利には、キャリアガス内の昇華されたタングステンヘキサカルボニル蒸気の飽和レベルが高くなる。更に、バッフル４１０を通る捻じれた流路は、有利には、前駆物質４１４の均一な消費と前駆物質ガスの生成のために前駆物質４１４の晒された表面積のほぼ全部がキャリアガスフローに晒される。   [0053] In one exemplary method of operation, the lower region 434 of the source canister 300 is at least partially filled with a mixture of tungsten hexacarbonyl and diffusion pump oil to form a slurry 412. The slurry 412 is maintained at a pressure of about 5 Torr and is heated to a temperature in the range of about 40 degrees Celsius to about 50 degrees Celsius by a resistance heater 430 near the source canister 300. Carrier gas in the form of argon flows through the inlet port 406 into the upper region 418 at a rate of about 400 standard cc / min. Prior to leaving the source canister 300 by the outflow port 408, the argon flows into an elongated average channel defined by the channel twisted by the baffle 410, preferably the average of argon in the upper region 418 of the source canister 300. Residence time is increased. The long residence time in the source canister 300 advantageously increases the saturation level of the sublimated tungsten hexacarbonyl vapor in the carrier gas. Further, the twisted flow path through the baffle 410 advantageously allows substantially all of the exposed surface area of the precursor 414 to be exposed to the carrier gas flow for uniform consumption of the precursor 414 and generation of precursor gas. It is.

[0054]図７は、前駆物質４１４を加熱するための他の実施形態を示すものである。更に詳しくは、図７はキャニスタヒータ７３０で取り囲まれたキャニスタ７００を示す断面図であり、キャニスタ７００の下部領域４３４とキャニスタ７００の上部領域４１８との間に温度勾配を生じるように構成され、下部領域４３４は最も低温の領域であり、上部領域４１８は最も高温の領域である。温度勾配は摂氏約５度〜摂氏約１５度の範囲にあってもよい。固体前駆物質が通常はキャニスタ７００の最も低温領域で蓄積又は凝縮する傾向があるので、キャニスタヒータ７３０は固体前駆物質４１４がキャニスタ７００の下部領域４３４に蓄積することを確実にするように構成され、それにより固体前駆物質４１４が凝縮するという予測性と固体前駆物質４１４の温度が高くなる。キャニスタヒータ７３０は、上部領域４１８及び下部領域４３４を含むキャニスタ７００全体がキャニスタヒータ７３０により加熱されるようにキャニスタヒータ７３０の内部に配置された加熱素子７５０を含んでいる。上部領域４１８近傍の加熱素子７５０は、下部領域４３４近傍の加熱素子７５０より高い熱を生成するように構成することができ、それによりキャニスタヒータ７３０が下部領域４３４と上部領域４１８間の温度勾配を生じることを可能にする。一実施形態においては、加熱素子７５０は上部領域４１８の温度が下部領域４３４の温度より摂氏約５度〜摂氏約１５度高いように構成される。他の実施形態においては、加熱素子７５０は上部領域４１８の温度が摂氏約７０度、下部領域４３４の温度が摂氏約６０度、キャニスタ７００の側壁の温度が摂氏約６５度であるように構成される。加熱素子７３０の電力は、２０８ＶＡＣ入力で約６００ワットとすることができる。   [0054] FIG. 7 illustrates another embodiment for heating the precursor 414. FIG. More specifically, FIG. 7 is a cross-sectional view showing a canister 700 surrounded by a canister heater 730, which is configured to generate a temperature gradient between a lower region 434 of the canister 700 and an upper region 418 of the canister 700. Region 434 is the coldest region and upper region 418 is the hottest region. The temperature gradient may be in the range of about 5 degrees Celsius to about 15 degrees Celsius. Since the solid precursor typically tends to accumulate or condense in the coldest region of the canister 700, the canister heater 730 is configured to ensure that the solid precursor 414 accumulates in the lower region 434 of the canister 700; This increases the predictability that the solid precursor 414 will condense and the temperature of the solid precursor 414. The canister heater 730 includes a heating element 750 disposed inside the canister heater 730 so that the entire canister 700 including the upper region 418 and the lower region 434 is heated by the canister heater 730. The heating element 750 near the upper region 418 can be configured to generate higher heat than the heating element 750 near the lower region 434 so that the canister heater 730 creates a temperature gradient between the lower region 434 and the upper region 418. Allows to occur. In one embodiment, the heating element 750 is configured such that the temperature of the upper region 418 is about 5 degrees Celsius to about 15 degrees Celsius above the temperature of the lower region 434. In other embodiments, the heating element 750 is configured such that the temperature of the upper region 418 is about 70 degrees Celsius, the temperature of the lower region 434 is about 60 degrees Celsius, and the temperature of the canister 700 sidewalls is about 65 degrees Celsius. The The power of the heating element 730 can be about 600 watts at 208 VAC input.

[0055]キャニスタヒータ７３０は、キャニスタ７００の最も低温の領域が下部領域４３４であることを更に確実にするためにキャニスタヒータ７３０の底面に位置する冷却プレート７２０を更に含み、それにより固体前駆物質４１４が下部領域４３４で凝縮することが確実である。冷却プレート７２０は、また、形が環状であってもよい。更に、バルブ３１２、３１４、オイルトラップ４５０、流入ポート４６０、流出ポート４０８は、抵抗加熱テープで加熱することができる。上部領域４１８は下部領域４３４より温度が高いように構成されるので、バッフル４１０は上部領域４１８から下部領域４３４に熱を伝達するために用いることができ、それによりキャニスタヒータ７３０が所望の温度勾配を維持することができる。   [0055] The canister heater 730 further includes a cooling plate 720 located on the bottom surface of the canister heater 730 to further ensure that the coldest region of the canister 700 is the lower region 434, thereby providing a solid precursor 414. Is surely condensed in the lower region 434. The cooling plate 720 may also be annular in shape. Further, the valves 312 and 314, the oil trap 450, the inflow port 460, and the outflow port 408 can be heated with resistance heating tape. Since the upper region 418 is configured to have a higher temperature than the lower region 434, the baffle 410 can be used to transfer heat from the upper region 418 to the lower region 434 so that the canister heater 730 can have a desired temperature gradient. Can be maintained.

[0056]図９は、キャニスタ７００の底部４３２から上部領域４１８まで伸びている複数のサイロ９１０を示す断面図である。図１０は、キャニスタ７００の底部４３２から上部領域４１８まで伸長したサイロ９１０を示す正面図である。サイロ９１０は前駆物質４１４の温度勾配を低減させるように構成され、それにより前駆物質内部の温度がほぼ均一になるように維持される。サイロ９１０は、底部４３２から前駆物質４１４と液体４１６の上面の少し上まで伸長することができる。サイロ９１０はポスト又はフィンの形であってもよい。サイロ９１０は、ステンレス鋼、アルミニウム等の熱伝導性物質から製造することができる。   FIG. 9 is a cross-sectional view illustrating a plurality of silos 910 extending from the bottom 432 of the canister 700 to the top region 418. FIG. 10 is a front view showing the silo 910 extending from the bottom 432 of the canister 700 to the upper region 418. The silo 910 is configured to reduce the temperature gradient of the precursor 414, thereby maintaining the temperature within the precursor substantially uniform. The silo 910 can extend from the bottom 432 to slightly above the top surfaces of the precursor 414 and the liquid 416. The silo 910 may be in the form of a post or fin. The silo 910 can be manufactured from a thermally conductive material such as stainless steel or aluminum.

[0057]図９は、更にソースキャニスタ７００の内容積４３８に配置される流入チューブ４２２を示す図である。チューブ４２２は、ソースキャニスタ７００の流入ポート４０６に第一端４２４で結合し、ソースキャニスタ７００の上部領域４１８における第二端４２６で終わる。チューブ４２２は、前駆物質４１４又はスラリー４１２の近い位置でソースキャニスタ７００の上部領域４１８にキャリアガスを注入する。第二端４２６は、更に、側壁４０２に向かってガスフローを送るように適合することができるので、ポート４０６、４０８間のキャニスタ７００を通ってガスの直接（直線又は透視線）フローを防止し、伸長した平均流路が生じる。   [0057] FIG. 9 further illustrates the inflow tube 422 disposed in the inner volume 438 of the source canister 700. FIG. Tube 422 is coupled to inflow port 406 of source canister 700 at first end 424 and ends at second end 426 in upper region 418 of source canister 700. The tube 422 injects a carrier gas into the upper region 418 of the source canister 700 near the precursor 414 or slurry 412. The second end 426 can further be adapted to direct gas flow toward the sidewall 402 to prevent direct (straight or perspective) flow of gas through the canister 700 between the ports 406, 408. An elongated average flow path results.

[0058]図５は、プロセスガスを生成するためのキャニスタ５００の他の実施形態を示す断面図である。キャニスタ５００は、内容積４３８を封入する側壁４０２、リッド４０４、底面４３２を含んでいる。リッド４０４又は側壁４０２の少なくとも１つが、ガス流入と流出のための流入ポート４０６と流出ポート４０８を含んでいる。キャニスタ５００の内容積４３８は上部領域４１８と下部領域４３４で分けられる。前駆物質４１４は少なくとも部分的に下部領域４３４を充填する。前駆物質４１４は固体、液体又はスラリーの形であってもよく、昇華又は気化によりプロセスガスを生成するよう適合されている。   [0058] FIG. 5 is a cross-sectional view illustrating another embodiment of a canister 500 for generating process gas. The canister 500 includes a side wall 402 that encloses an internal volume 438, a lid 404, and a bottom surface 432. At least one of the lid 404 or the side wall 402 includes an inflow port 406 and an outflow port 408 for gas inflow and outflow. The internal volume 438 of the canister 500 is divided into an upper region 418 and a lower region 434. Precursor 414 at least partially fills lower region 434. The precursor 414 may be in the form of a solid, liquid or slurry and is adapted to produce a process gas by sublimation or vaporization.

[0059]チューブ５０２はキャニスタ５００の内容積４３８内に配置され、前駆物質からキャニスタ５００内にガスフローを送るように適合され、有利にはチューブ５０２から流れるガスが前駆物質４１４に直接衝突することや微粒子が空気によって運ばれることを防止し、流出ポート４０８を通ってプロセスチャンバ３０６に運ばれる。チューブ５０２は第一端５０４で流入ポート４０６に結合されている。チューブ５０２は、第一端５０４から前駆物質４１４の上の上部領域４１８に位置する第二端５２６Ａに伸びている。第二端５２６Ａは側壁４０２に向かってガスフローを送るように適合されてもよいので、ポート４０６、４０８間のキャニスタ５００を通ってガスの直接フロー（直線又は透視線）を防止し、伸長した平均流路が生じる。   [0059] The tube 502 is disposed within the interior volume 438 of the canister 500 and is adapted to send a gas flow from the precursor into the canister 500, preferably the gas flowing from the tube 502 impinges directly on the precursor 414. And particulates are prevented from being carried by the air and are carried through the outflow port 408 to the process chamber 306. Tube 502 is coupled to inflow port 406 at a first end 504. Tube 502 extends from a first end 504 to a second end 526A located in the upper region 418 above the precursor 414. The second end 526A may be adapted to route gas flow toward the side wall 402, thus preventing direct flow of gas (straight line or perspective) through the canister 500 between the ports 406, 408 and extended. An average flow path is created.

[0060]一実施形態においては、チューブ５０２の第二端５２６Ａの流出口５０６は、キャニスタ５００の中心軸５０８に相対して約１５〜９０度の角度に向いている。他の実施形態においては、チューブ５０２は流出口５０６を出るガスフローをキャニスタ５００のリッド４０４に送る、‘Ｊ’型の第二端５２６Ｂを有する。他の実施形態においては、チューブ５０２はチューブ５０２の端の近くにプラグ又はキャップ５１０を有する、キャップ構造の第二端５２６Ｃを有する。キャップ構造の第二端５２６Ｃは、キャップ５１０の近くのチューブ５０２の側面に形成される少なくとも一つの開口５２８を有する。開口５２８を出るガスは、典型的に中心軸５０８に対して垂直に、キャニスタ５００の下部領域４３４に配置される前駆物質４１４から送られる。任意に、上記のような少なくとも１つのバッフル４１０（想像線で示されている）はチャンバ５００内に配置することができ、上記チューブ５０２の実施形態のいずれかと縦に並べて用いることができる。   [0060] In one embodiment, the outlet 506 of the second end 526A of the tube 502 is oriented at an angle of about 15-90 degrees relative to the central axis 508 of the canister 500. In other embodiments, the tube 502 has a 'J' shaped second end 526B that directs the gas flow exiting the outlet 506 to the lid 404 of the canister 500. In other embodiments, the tube 502 has a second end 526C of the cap structure having a plug or cap 510 near the end of the tube 502. The second end 526C of the cap structure has at least one opening 528 formed in the side of the tube 502 near the cap 510. Gas exiting the opening 528 is delivered from a precursor 414 disposed in the lower region 434 of the canister 500, typically perpendicular to the central axis 508. Optionally, at least one baffle 410 (shown in phantom) as described above can be placed in chamber 500 and used in tandem with any of the embodiments of tube 502 described above.

[0061]一例示的動作方式においては、キャニスタ５００の下部領域４３４は、スラリー４１２を形成するためにタングステンヘキサカルボニルと拡散ポンプオイルの混合物で少なくとも部分的に充填される。スラリー４１２は約５Ｔｏｒｒの圧力に保たれ、キャニスタ５００近くにある抵抗ヒータ４３０によって約４０〜摂氏約５０度の範囲の温度に加熱される。アルゴンの形のキャリアガスは、約２００標準ｃｃ/ｍｉｎの速度で上部領域４１８に流入ポート４０６とチューブ５０２によって流れる。チューブ５０２の第二端５２６Ａは、流出ポート４０８から離れた伸長された平均流路にキャリアガスのフローを送り、有利にはキャニスタ５００の上部領域４１８におけるアルゴンの平均滞留時間が長くなり、微粒子生成を最少にするために前駆物質４１４上のキャリアガスの直接フローを防止する。微粒子生成の低減により製品歩留まりが改善され、供給源固形物を保存し、下流での汚染が減少するが、キャニスタ５００における滞留時間の増加は、有利には、キャリアガス内の昇華したタングステンヘキサカルボニルガスの飽和レベルを増大させる。   [0061] In one exemplary mode of operation, the lower region 434 of the canister 500 is at least partially filled with a mixture of tungsten hexacarbonyl and diffusion pump oil to form a slurry 412. The slurry 412 is maintained at a pressure of about 5 Torr and is heated to a temperature in the range of about 40 to about 50 degrees Celsius by a resistance heater 430 near the canister 500. A carrier gas in the form of argon flows into the upper region 418 through the inlet port 406 and the tube 502 at a rate of about 200 standard cc / min. The second end 526A of the tube 502 directs the carrier gas flow to an elongated average flow path away from the outflow port 408, advantageously increasing the average residence time of argon in the upper region 418 of the canister 500 and generating particulates. To prevent direct flow of carrier gas over precursor 414. Although reduced product formation improves product yield and preserves source solids and reduces downstream contamination, increased residence time in the canister 500 is advantageously sublimated tungsten hexacarbonyl in the carrier gas. Increase gas saturation level.

[0062]図６は、前駆物質ガスを生成するためのキャニスタ６００の他の実施形態を示す断面図である。キャニスタ６００は内容積４３８を封入する側壁４０２、リッド４０４、底面４３２を含んでいる。リッド４０４又は側壁４０２の少なくとも１つは、ガス流入と流出のために流入ポート４０６と流出ポート４０８を有する。流入ポートと流出ポート４０６、４０８は、ガス分配システム３０４からキャニスタ６００の取り外しを容易にするために一対の切断取付け具４３６Ａ、４３６Ｂを備えたバルブ３１２、３１４に結合されている。任意に、プロセスチャンバに流れているガスに存在することができるあらゆるオイル粒子を捕捉するために、流出ポート４０８とバルブ３１４間にオイルトラップ４５０が結合されている。   [0062] FIG. 6 is a cross-sectional view illustrating another embodiment of a canister 600 for generating a precursor gas. The canister 600 includes a side wall 402 that encloses an internal volume 438, a lid 404, and a bottom surface 432. At least one of the lid 404 or the side wall 402 has an inflow port 406 and an outflow port 408 for gas inflow and outflow. Inlet and outlet ports 406, 408 are coupled to valves 312, 314 with a pair of cutting fixtures 436 A, 436 B to facilitate removal of canister 600 from gas distribution system 304. Optionally, an oil trap 450 is coupled between the outflow port 408 and the valve 314 to trap any oil particles that may be present in the gas flowing into the process chamber.

[0063]キャニスタ６００の内容積４３８は、上部領域４１８と下部領域４３４に分けられる。前駆物質４１４と液体４１６は、少なくとも部分的に下部領域４３４を充填する。チューブ６０２はキャニスタ６００の内容積４３８に配置され、前駆物質と液体混合体から離れてキャニスタ６００内に第一ガスフローＦ1を送るように、また、混合物によって第二ガスフローＦ2を送るように適合されている。フローＦ1はフローＦ2よりかなり大きい。フローＦ2はバブラーとして作用するよう構成され、前駆物質と液体混合物を攪拌するのに十分であるが、前駆物質４１４又は液体４１６の微粒子又は小滴が空気によって運ばせるには十分でない。従って、この実施形態は、有利には、チューブ６０２から流れるガスの直接の衝突のために生じ流出ポート４０８を通って処理チャンバ３０６に運ばれる微粒子を最少にしつつ前駆物質と液体混合物を攪拌する。 [0063] The internal volume 438 of the canister 600 is divided into an upper region 418 and a lower region 434. Precursor 414 and liquid 416 at least partially fill lower region 434. The tube 602 is disposed in the internal volume 438 of the canister 600 to send the first gas flow F 1 into the canister 600 away from the precursor and liquid mixture, and to send the second gas flow F 2 through the mixture. It is adapted to. Flow F 1 is much larger than flow F 2 . Flow F 2 is configured to act as a bubbler and is sufficient to agitate the precursor and liquid mixture, but not enough to cause particulates or droplets of precursor 414 or liquid 416 to be carried by the air. Thus, this embodiment advantageously stirs the precursor and liquid mixture while minimizing particulates that are generated by direct impingement of the gas flowing from the tube 602 and carried through the outflow port 408 to the processing chamber 306.

[0064]チューブ６０２は第一端６０４で流入ポート４０６に結合される。チューブ６０２は、第一端６０４から、前駆物質と液体混合体内の、キャニスタ６００の下部領域４３４に位置する第二端６０６まで伸びている。チューブ６０２は、第一ガスフローＦ1をキャニスタ６００の側壁４０２に対して送るキャニスタ６００の上部領域４１８に配置された開口６０８を有する。チューブ６００は、開口部６０８の下にあるキャニスタ６００の上の領域４３８に配置された制限部６１０を有する。制限部６１０は、チューブ６０２の第二端６０６からスラリー４１２に対して流れる第二ガスフローＦ2を減少させるように働く。制限部の量を調節することにより、第一ガスフローと第二ガスフローＦ1とＦ2の相対的な速度が調節され得る。この調節は少なくとも２つのためにある。第一に、プロセスチャンバ３０６の微粒子生成や潜在的な汚染を最少にしつつ、第二ガスフローＦ2が液体４１６中の前駆物質４１４の懸濁又は混合を維持するのに十分なだけ攪拌するように最少にされ得る。第二に、第一ガスフローＦ1が必要とされる量の昇華及び/又は蒸気を前駆物質４１４からプロセスチャンバ３０６へ供給するのに必要な全体のフロー体積を維持するために調節され得る。 [0064] Tube 602 is coupled to inflow port 406 at a first end 604. The tube 602 extends from a first end 604 to a second end 606 located in the lower region 434 of the canister 600 in the precursor and liquid mixture. The tube 602 has an opening 608 disposed in the upper region 418 of the canister 600 that sends the first gas flow F 1 to the side wall 402 of the canister 600. Tube 600 has a restriction 610 located in region 438 above canister 600 below opening 608. The restrictor 610 serves to reduce the second gas flow F 2 flowing from the second end 606 of the tube 602 to the slurry 412. By adjusting the amount of the restriction, the relative speeds of the first gas flow and the second gas flows F 1 and F 2 can be adjusted. This adjustment is for at least two. First, the second gas flow F 2 is agitated enough to maintain the suspension or mixing of the precursor 414 in the liquid 416 while minimizing particulate formation and potential contamination in the process chamber 306. Can be minimized. Second, the first gas flow F 1 can be adjusted to maintain the overall flow volume required to supply the required amount of sublimation and / or vapor from the precursor 414 to the process chamber 306.

[0065]任意に、上記のような少なくとも１つのバッフル４１０はキャニスタ６００内に配置されてもよく、上記チューブ６０２の実施形態のいずれかと縦に用いてもよい。   [0065] Optionally, at least one baffle 410 as described above may be disposed within the canister 600 and may be used vertically with any of the embodiments of the tube 602 described above.

[0066]前述は本発明の好適実施形態に関するが、更に多くの本発明の実施形態が本発明の基本的な範囲から逸脱することなく構成されてもよく、その範囲は以下の特許請求の範囲によって決定される。   [0066] While the foregoing relates to preferred embodiments of the invention, many more embodiments of the invention may be made without departing from the basic scope of the invention, the scope of which is set forth in the following claims Determined by.

図１は、原子層堆積（ＡＬＤ）により基板上に形成されたバリヤ層の一実施形態の概略断面図である。FIG. 1 is a schematic cross-sectional view of one embodiment of a barrier layer formed on a substrate by atomic layer deposition (ALD). 図２Ａは、基板の例示的な部分にタンタル含有化合物の単層の化学吸着を示す一実施形態である。FIG. 2A is an embodiment showing monolayer chemisorption of a tantalum-containing compound on an exemplary portion of the substrate. 図２Ｂは、基板の例示的な部分にタンタル含有化合物と窒素含有化合物の単層の化学吸着を示す一実施形態である。FIG. 2B is one embodiment showing a single layer chemisorption of a tantalum-containing compound and a nitrogen-containing compound on an exemplary portion of the substrate. 図２Ｃは、基板の例示的な部分にタンタル含有化合物と窒素含有化合物の単層の交互化学吸着を示す一実施形態である。FIG. 2C is an embodiment showing alternating chemisorption of monolayers of tantalum-containing and nitrogen-containing compounds on an exemplary portion of the substrate. 図３は、原子層堆積によって１以上のバリヤ層を形成するために用いることができる処理システムの例示的な一実施形態の概略断面図である。FIG. 3 is a schematic cross-sectional view of an exemplary embodiment of a processing system that can be used to form one or more barrier layers by atomic layer deposition. 図４Ａは、ガス生成キャニスタの一実施形態の側断面図である。FIG. 4A is a side cross-sectional view of one embodiment of a gas generation canister. 図４Ｂは、図４Ａのガス生成キャニスタの正面断面図である。4B is a front cross-sectional view of the gas generating canister of FIG. 4A. 図５は、ガス生成キャニスタの他の実施形態の断面図である。FIG. 5 is a cross-sectional view of another embodiment of a gas generating canister. 図６は、ガス生成キャニスタの他の実施形態の側断面図である。FIG. 6 is a side cross-sectional view of another embodiment of a gas generating canister. 図７は、本発明の一実施形態のキャニスタヒータに取り囲まれたキャニスタを示す断面図である。FIG. 7 is a cross-sectional view showing a canister surrounded by a canister heater according to an embodiment of the present invention. 図８は、本発明の一実施形態の複数の固体粒子を含有するキャニスタを示す断面図である。FIG. 8 is a cross-sectional view showing a canister containing a plurality of solid particles according to an embodiment of the present invention. 図９は、本発明の一実施形態のキャニスタの底部から上の領域に伸びている複数のサイロを示す断面図である。FIG. 9 is a cross-sectional view showing a plurality of silos extending from the bottom to the upper region of the canister according to one embodiment of the present invention. 図１０は、本発明の一実施形態のキャニスタの底部から上の領域に伸びている複数のサイロを示す正面図である。FIG. 10 is a front view showing a plurality of silos extending from a bottom portion to an upper region of a canister according to an embodiment of the present invention.

符号の説明Explanation of symbols

１００…基板、１０２…誘電体層、１０４…バリヤ層、１５０…基板構造、２００…基板、２０５…タンタル含有化合物、２１０…タンタル原子、２１５…反応性化学種、２２５…窒素含有化合物、２３５…反応性化学種、３００…ソースキャニスタ、３０２…キャリアガス源、３０４…ガス分配システム、３０６…処理チャンバ、３１０…フローコントローラ、３１２、３１４…バルブ、３２０…処理システム、４０２…側壁、４０４…リッド、４０６…流入ポート、４０８…流出ポート、４１０…バッフル、４１２…スラリー、４１４…前駆物質、４１６…液体、４１８…上の領域、４２０…ハウジング、４２２…チューブ、４３２…底部、４３４…下の領域、４３６…切断取付け具、４３８…内容積、４４０…磁気スターラー、４４４…磁気ピル、４５０…オイルトラップ、４５２…本体、５００…キャニスタ、５２８…開口、６００…キャニスタ、７００…キャニスタ、７２０…冷却プレート、７３０…キャニスタヒータ、７５０…加熱素子、８００…キャニスタ、８１０…固体粒子。   DESCRIPTION OF SYMBOLS 100 ... Substrate, 102 ... Dielectric layer, 104 ... Barrier layer, 150 ... Substrate structure, 200 ... Substrate, 205 ... Tantalum-containing compound, 210 ... Tantalum atom, 215 ... Reactive chemical species, 225 ... Nitrogen-containing compound, 235 ... Reactive species, 300 ... Source canister, 302 ... Carrier gas source, 304 ... Gas distribution system, 306 ... Processing chamber, 310 ... Flow controller, 312, 314 ... Valve, 320 ... Processing system, 402 ... Side wall, 404 ... Lid 406 ... Inlet port, 408 ... Outlet port, 410 ... Baffle, 412 ... Slurry, 414 ... Precursor, 416 ... Liquid, 418 ... Upper region, 420 ... Housing, 422 ... Tube, 432 ... Bottom, 434 ... Below Area 436 ... Cutting fixture 438 ... Internal volume 440 ... Magnetic stirrer 444 Magnetic pill, 450 ... Oil trap, 452 ... Main body, 500 ... Canister, 528 ... Opening, 600 ... Canister, 700 ... Canister, 720 ... Cooling plate, 730 ... Canister heater, 750 ... Heating element, 800 ... Canister, 810 ... Solid particle.

Claims (17)

基板上の１以上の特徴部を充填する方法であって、
ソースキャニスタを、ソースキャニスタの上側部分と、精製ペンタキス（ジメチルアミド）タンタルを部分的に充填された該ソースキャニスタの下側部分との間で、上側部分が下側部分よりも高温となる温度勾配を生じるように加熱素子で加熱し、底部から伸びている複数のサイロにより前記下側部分に充填されている精製ペンタキス（ジメチルアミド）タンタルの温度勾配を低減することで該精製ペンタキス（ジメチルアミド）タンタルの内部温度をほぼ均一になるように維持するステップと、
該ソースキャニスタから精製ペンタキス（ジメチルアミド）タンタルを前記加熱することにより生成した前駆物質ガスを基板に送り、さらに窒素含有化合物を基板へ送って該基板上に窒化タンタルバリヤ層を堆積させるステップであって、該バリヤ層が全不純物の合計が５ｐｐｍ未満である精製ペンタキス(ジメチルアミド)タンタル及び窒素含有化合物の熱分解生成物である窒化タンタルから形成される、前記ステップと、
該バリヤ層上にシード層を堆積させるステップと、
該シード層上に導電層を堆積させるステップと、
を含む、前記方法。 A method of filling one or more features on a substrate, comprising:
A temperature gradient between the source canister and the upper part of the source canister and the lower part of the source canister partially filled with purified pentakis (dimethylamido) tantalum, the upper part being hotter than the lower part The purified pentakis (dimethylamide) is heated by a heating element so as to produce a temperature gradient of the purified pentakis (dimethylamido) tantalum filled in the lower portion by a plurality of silos extending from the bottom. Maintaining the internal temperature of tantalum to be substantially uniform;
There in depositing the generated precursor gas feed into the substrate, a tantalum nitride barrier layer on the substrate further sending a nitrogen-containing compound to the substrate by the heating purified pentakis (dimethylamido) tantalum from said source canister Te, the barrier layer is Ru is formed from tantalum nitride is thermal decomposition product of the sum is less than 5ppm purified pentakis (dimethylamido) tantalum and nitrogen-containing compounds of all impurities, and the step,
Depositing a seed layer on the barrier layer;
Depositing a conductive layer on the seed layer;
Said method. 前記精製ペンタキス（ジメチルアミド）タンタルは、ペンタキス（ジメチルアミド）タンタルを昇華してタンタルオキソアミドの少なくとも一部が除去されたものである、請求項１記載の方法。 The method according to claim 1 , wherein the purified pentakis (dimethylamido) tantalum is obtained by sublimating pentakis (dimethylamido) tantalum to remove at least a part of tantalum oxoamide . 該導電層が銅を含んでいる、請求項１記載の方法。   The method of claim 1, wherein the conductive layer comprises copper. 該バリヤ層が原子層堆積により形成される、請求項１記載の方法。   The method of claim 1, wherein the barrier layer is formed by atomic layer deposition. 該不純物が、塩素、リチウム、鉄、フッ素、臭素、ヨウ素、及びその組合わせからなる群より選ばれる、請求項１記載の方法。   The method of claim 1, wherein the impurity is selected from the group consisting of chlorine, lithium, iron, fluorine, bromine, iodine, and combinations thereof. 精製ペンタキス(ジメチルアミド)タンタルを用いてバリヤ層を堆積させることにより、未精製ペンタキス(ジメチルアミド)タンタルを用いて形成されたバリヤ層上に形成された導電層より欠陥が少ない導電層が得られる、請求項１記載の方法。 Depositing a barrier layer using purified pentakis (dimethylamido) tantalum provides a conductive layer with fewer defects than the conductive layer formed on the barrier layer formed using unpurified pentakis (dimethylamido) tantalum. The method of claim 1. 基板上に窒化タンタルバリヤ層を堆積させる方法であって、
基板がその中に配置された処理チャンバに、ソースキャニスタを加熱して生成した前駆体ガスを流して、該基板上にタンタル含有層を形成するステップであって、該精製ペンタキス(ジメチルアミド)タンタルが全不純物の合計が５ｐｐｍ以下であり、前記ソースキャニスタを、その上側部分と精製ペンタキス（ジメチルアミド）タンタルが部分的に充填された該ソースキャニスタの下側部分との間で、上側部分が下側部分よりも高温となる温度勾配を生じるように加熱素子により加熱し、該ソースキャニスタの底部から伸びている複数のサイロにより前記下側部分に充填されている精製ペンタキス（ジメチルアミド）タンタルの温度勾配を低減することで該精製ペンタキス（ジメチルアミド）タンタルの内部温度をほぼ均一になるように維持する前記ステップと、
該処理チャンバに窒素含有化合物を導入して該基板上に窒素含有層を形成するステップと、
を含む、前記方法。 A method of depositing a tantalum nitride barrier layer on a substrate, comprising:
Flowing a precursor gas generated by heating a source canister into a processing chamber in which the substrate is disposed to form a tantalum-containing layer on the substrate, the purified pentakis (dimethylamido) tantalum The total impurity is 5 ppm or less, and the source canister is placed between its upper part and the lower part of the source canister partially filled with purified pentakis (dimethylamido) tantalum, The temperature of purified pentakis (dimethylamido) tantalum that is heated by a heating element so as to generate a temperature gradient that is higher than that of the side portion, and is filled in the lower portion by a plurality of silos extending from the bottom of the source canister Maintaining the internal temperature of the purified pentakis (dimethylamido) tantalum to be almost uniform by reducing the gradient Said the step that,
Introducing a nitrogen-containing compound into the processing chamber to form a nitrogen-containing layer on the substrate;
Said method. 該基板の温度が１００℃〜３００℃である、請求項７記載の方法。 The method according to claim 7, wherein the temperature of the substrate is 100 ° C. to 300 ° C. 該処理チャンバの圧力が１．０〜５．０Ｔｏｒｒである、請求項７記載の方法。 The method of claim 7, wherein the pressure in the processing chamber is 1.0 to 5.0 Torr . 該不純物が、本質的に、塩素、リチウム、鉄、フッ素、臭素、ヨウ素、及びその組合わせからなる群より選ばれる、請求項７記載の方法。   The method of claim 7, wherein the impurities are selected from the group consisting essentially of chlorine, lithium, iron, fluorine, bromine, iodine, and combinations thereof. 該窒素含有化合物がアンモニアガスを含んでいる、請求項７記載の方法。   The method of claim 7 wherein the nitrogen-containing compound comprises ammonia gas. 該窒素含有化合物が、アンモニア、ヒドラジン、ジメチルヒドラジン、ｔ-ブチルヒドラジン、フェニルヒドラジン、２,２-アゾイソブタン、エチルアジド、その誘導体、及びその組合わせからなる群より選ばれる、請求項７記載の方法。   8. The method of claim 7, wherein the nitrogen-containing compound is selected from the group consisting of ammonia, hydrazine, dimethyl hydrazine, t-butyl hydrazine, phenyl hydrazine, 2,2-azoisobutane, ethyl azide, derivatives thereof, and combinations thereof. . 該バリヤ層が原子層堆積によって形成される、請求項７記載の方法。   The method of claim 7, wherein the barrier layer is formed by atomic layer deposition. 該基板の温度が、該バリヤ層堆積の５０％以上が化学吸着によるように選ばれる、請求項７記載の方法。   The method of claim 7, wherein the temperature of the substrate is selected such that 50% or more of the barrier layer deposition is due to chemisorption. 該基板上に該タンタル含有層を形成するステップにおいて、該処理チャンバに導入する前に該精製ペンタキス(ジメチルアミド)タンタルが前記ソースキャニスタ内で昇華される、請求項７記載の方法。 8. The method of claim 7 , wherein in the step of forming the tantalum-containing layer on the substrate , the purified pentakis (dimethylamido) tantalum is sublimed in the source canister prior to introduction into the processing chamber. 該基板上に該タンタル含有層を形成する際に、該精製ペンタキス(ジメチルアミド)タンタルが基板上に化学吸着された後、チャンバー内の過剰な該ペンタキス(ジメチルアミド)タンタルを除去するステップを更に含む、請求項７記載の方法。 In forming the tantalum-containing layer on the substrate, after the purified pentakis (dimethylamido) tantalum is chemisorbed on the substrate, the step of removing excess pentakis (dimethylamido) tantalum in the chamber is further included. 8. The method of claim 7, comprising. 請求項１或いは請求項２に記載の方法に用いられる、全不純物の合計が５ｐｐｍ以下である精製ペンタキス(ジメチルアミド)タンタルを含有する前駆物質を含むソースキャニスタであって、
該不純物が、タンタルオキソアミド、塩素、リチウム、鉄、フッ素、臭素、ヨウ素、及びその組合わせからなる群より選ばれ、
前記ソースキャニスタを加熱素子により加熱してその内部に上側部分が下側部分よりも高温となる温度勾配を生じさせ、
前記ソースキャニスタが、前記下側部分に充填される前駆物質の温度勾配を低減することで該精製ペンタキス(ジメチルアミド)タンタルの内部温度をほぼ均一になるように維持するために該ソースキャニスタの底部から伸びている複数のサイロを備えている、前記ソースキャニスタ。 A source canister comprising a precursor containing purified pentakis (dimethylamido) tantalum , used in the method according to claim 1 or claim 2, wherein the sum of all impurities is 5 ppm or less,
The impurities are selected from the group consisting of tantalum oxoamide, chlorine, lithium, iron, fluorine, bromine, iodine, and combinations thereof;
The source canister is heated by a heating element to generate a temperature gradient in which the upper part is hotter than the lower part .
The source canister has a bottom portion of the source canister to maintain a substantially uniform internal temperature of the purified pentakis (dimethylamido) tantalum by reducing the temperature gradient of the precursor filling the lower portion. The source canister comprising a plurality of silos extending from the source canister.
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