TW567544B - Method and apparatus for depositing tungsten after surface treatment to improve film characteristics - Google Patents

Method and apparatus for depositing tungsten after surface treatment to improve film characteristics Download PDF

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TW567544B
TW567544B TW091115883A TW91115883A TW567544B TW 567544 B TW567544 B TW 567544B TW 091115883 A TW091115883 A TW 091115883A TW 91115883 A TW91115883 A TW 91115883A TW 567544 B TW567544 B TW 567544B
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tungsten
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Jeong-Soo Byun
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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
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • C23C16/0281—Deposition of sub-layers, e.g. to promote the adhesion of the main coating of metallic sub-layers
    • 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
    • C23C16/08—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 metal halides
    • C23C16/14—Deposition of only one other metal element
    • 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]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
    • C23C16/45529—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making a layer stack of alternating different compositions or gradient compositions
    • 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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 Table
    • 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 Table 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
    • 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
    • H01L21/76871—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers
    • H01L21/76876—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers for deposition from the gas phase, 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
    • H01L21/70—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
    • H01L21/76877—Filling of holes, grooves or trenches, e.g. vias, with conductive material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2221/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof covered by H01L21/00
    • H01L2221/10—Applying interconnections to be used for carrying current between separate components within a device
    • H01L2221/1068—Formation and after-treatment of conductors
    • H01L2221/1073—Barrier, adhesion or liner layers
    • H01L2221/1084—Layers specifically deposited to enhance or enable the nucleation of further layers, i.e. seed layers
    • H01L2221/1089—Stacks of seed layers

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
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  • Chemical Vapour Deposition (AREA)
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  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)

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567544 A7 B7 五、發明説明（） 發明領域： 本發明之實施例與半導體基材的處理有關。更詳而 言之’本發明之實施例係關於半導體基材上沉積耐熱金 屬層製程的改善。 發明背景： 半導體製造業所追求者不外於提升較大基材上沉積 層膜之均勻性的同時得到更高的生產良率，其提升因素 及新材料的提出同樣亦能使基材上單位面積上電路密度 增南。隨著電路密度的增加，在層膜厚度增加時均勻度 及製程控制的精準度亦隨之增加。因此，現已開發出多 種在基材上行較低成本沉積之技術，此等技術同時能維 持對層膜特性控制之能力。CVD為一種與通量相關之沉 積技術’其需對基材溫度及通入處理室之前驅物提供精 準控制，藉以生成均勻厚度層膜。隨著基材的增大（如自 直徑2 0 0毫米提升至直徑3 〇 〇毫米），這些控制要件變得 格外重要，故為維持均句度，處理室設計及氣流技術便 變得更加複雜。 原子層沉積（ALD)是一種C VD技術的變形，其能表 現出優異的步階覆蓋特性。ALD之沉積原理為原子層磊 晶（ALE)技術，其中ALE技術為原先電激光顯示器製造 所用者。ALD利用化學吸收作用而沉積一反應前驅物分 子飽和單層於一基材表面上，其達成方式為使一適用反 應前驅物以間歇形成脈衝量之方式送進一沉積室中，其 第5頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) (請先閲讀背面之注意事項再填寫本頁) 、一占 經濟部智慧財產局員Η消費合作社印製 567544 A7 B7 五、發明說明（） 中一反應前驅物的每一次注入為一不活潑氣體清洗氣流 所隔開，藉以在先前沉積完之層膜上供以被吸收原子 層。此動作重覆進行，直至於該基材上均勻層膜達至所 需厚度。不過，ALD技術仍有沉積速率遠低於一般CVD 技術之憾，其間至少相差一數量級。 高逮下沉積層膜、且該膜層需提供良好的步階覆蓋 結果乃是互相衝突的，一般作法通常為犧牲一者而保全 另一者。對於形成介電層間金屬層之内連接接觸洞形成 期間耐熱今屬材料沉積於孔洞之上的製程而言，這種衝 突格別明顯。長久以來，CVD技術用於導電材料（如耐熱 金屬材料）之沉積，藉以利用低成本及快速之方式完成孔 洞之填充。由於半導體電路密度的增加，鎢已因其優異 之步階覆蓋特性而被選用為填充此等高寬高比結構之材 料。因此，鎢之化學氣相沉積得因高產率及良好步階覆 蓋特性而廣泛應用於半導體製造界中。 然而，以傳統CVD法沉積鎢卻有數個缺點。舉例而 言’當沉積溫度低於400°C時，半導體晶圓鎢彼覆層的 沉積相當耗時。此種耗時沉積得因增高沉積溫度而得到 改善’如可增至約500°c至5 5 0°c。然而，於此種高溫下 沉積’製造中積體電路下層部份的結構及操作一致性可 能受損。另則，鎢沉積形成之表面粗糙，這使得製造時 微影步驟的進行變得較複雜，其中鎢所形成之表面的反 射率僅為矽表面者之20%(甚小於20%)。最後，鶴之沉 積均勻度不佳，其膜層厚度差約1 %，其膜層之阻抗控制 第6頁 本紙張尺度適用中國國家標準(CNS)A4規格(210x297公釐) (請先閲讀背面之注意事項再填寫本頁) 、\π- 經濟部智慧財產局員工消費合竹相却架 567544 A 7 五、發明説明（ 能力因此不佳。針對μ、+ … 十對上述缺點’先前已有多種應變措施 的提出。 舉例而言，張蓉人4也 〇 人所擁有之美國專和！ 5,028,565即 揭路一種利用改變沉籍仆與 文，儿積化學條件而改善鎢膜均 法，該專利與本發明之爲嘈乂 ▲ 又 月之文讓人為同者。就相關方面言， 該方法包含塊體沉穑较瞭二#上 帛鶴膜刖於中間阻障層上形成一孕核 層之步驟，其中孕核層撂與也# e 層侍棱供成長位置、藉以提升其上 層鎮膜之均勻度，其形成係由丄 珉係由/、鼠化鎢、氧、矽烷及氬 組成之氣體混合物所達成。此 午孩層具與阻障層相 關之優點：舉例而言，芒LV备儿&仏上 ° 右以虱化鈦作為阻障層時，鎢層 的厚度均勻度得提升15%之多以 曰 ， 夕1一右以濺鍍鎢或濺鍍鎢 化鈦為阻障材料時’孕核層所帶來的效益仍未有說明。 故而’得提升半導體基材上沉積之奈熱性金屬層特 性之技術確又其提出之必要。 發明目的及概沭： 一種於一基材上形成一耐熱金屬層之方法及系統，其 中包含加入還原劑、並於之後加入含鎢化合物以形成鎢層 之步驟，其中還原劑可為PI或B^6等，而鎢化合物得 為WF0等。本案發明人相信鎢膜特性之提升有助於還原劑 及含鎢化合物間之化學親合性，藉以改善經吸收之化學物 質的表面移動能力，並能提升WF0於鎢膜處於孕核階段時 之還原能力。 該方法可更包含續加入一還原劑及一含鎢化合物以 本紙張尺度適用中國國家標準(CNS)A4規格(210x297公釐) (請先閲讀背面之注意事項再填寫本頁) 、可. 經濟部智慧財產局員工消費合作社印製 567544 A 7
匕積鶴膜之步驟， q層原劑得為叫或b2h6。戶斤 或也可用以拮 丁鬼材鎢層沉積前的孕核 』用以填充孔洞。 層 經濟部智慧財產局員工消費合作社印製 第1圖為本發明一丰導體處 ^ 0 ^ , 牛V體处里糸統一實施例之前視圖。 圖為第1圖之處理室一實A #， 貫％例的剖面示意圖。 第3圖為為— 基材之剖面7"意、圖，其中顯示後續沉積時 基材上一還原劑之可能吸附機制。 Θ為為基材之剖面視意圖，其中顯示該還原劑加 後基材上方之含耐熱金屬化合物的可能能吸附 制。 第5圖為—處理室中存在氣體的濃度圖，其中該處理室 為第2圖所示之處理室。 第6圖顯示本發明+ ALD循環次數及利用後續沉積方 在一基材上形成之一層之厚度間的關係。 第7圖顯示本發明中後續沉積循環次數及利用後續沉積 式在一基材上形成之一層之阻抗間的關係。 第8圖顯示利用後續沉積方式在一基材上形成之一層之沉 積速率與基材溫度間的關係。 第9圖顯示本發明中利用後續沉積方式在一基材上形 一層之阻抗與基材溫度間的關係。 第10圖為本發明中一經圖案化之基材實施例的剖面 圖，其中該基材上以後續沉積技術形成一孕核層 第8頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) (請先間讀背面之法意-#項#瑱·:s本頁) 入 式 方 成之 示意 567544 A7 B7 五、發明説明（） 第1 1圖為第1 0圖之一基材實施例的剖面示意圖，其中尚 有一耐熱金屬層以CVD方式形成於孕核層之上。 第1 2圖顯示本發明另一實施例中一處理室中存在之氣體 濃度，其中該處理室得為第2圖所示之處理室。 第1 3圖顯示本發明另一實施例中一處理室中存在之氣體 濃度，其中該處理室得為第2圖所示之處理室。 第1 4圖顯示氟含量與一基材上以ALD技術形成之一耐熱 金屬層深度間的關係圖，其中係以氬或氮為載氣。 第15圖為顯示氟含量與一基材上以ALD技術形成之一耐 熱金屬層深度間的關係圖，其中係以氫為載氣。 第16圖為本發明一實施例中第3圖及第4圖上之一基材 實施例的一剖面示意圖，在該基材上有一層PH3或 B2H6形成於該基材及一鎢層之間。 第1 7圖為本發明一實施例中一處理室存在之氣體的濃度 圖，其中該處理室可為第2圖所示之處理室。 第1 8圖為第3圖及第4圖之一基材實施例的剖面示意圖， 其中一含鈦層夾於一基材及一 PH3或B2H6層之 間，此為本發明所建構者。 圖號對照說明： 12 處理室 14 處理室 16 共同工作區 18 牆 22 控制器 24 監視器 26 監視器 28 光筆 第9頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) (請先閲讀背面之注意事項再填寫本頁) 、V'V7· 經濟部智慧財產局員工消費合作社印製 567544 A7 B7 五、發明説明（） 30 機 殼 32 底 部 牆 34 蓋 件 36 側 壁 37 處 理 室 38 座 檯 39 光 筆 39a, ,39b ,39c 處 理 氣體 41 流 量 閥 42 基 材 43 交 流 電 源 供 應 器 44 加 熱 零 件 46 溫 度 感 測 器 48 真 空 幫 浦 60 孕 核 層 61 阻 障 層 63 孔 洞 70 層 膜 72 鎢 層 76 晶 圓 90 中 央 處 理 記 憶 體 92 隨 機 存 取 記 憶 體 (請先閲讀背面之注意事項再填窍本頁) 、ρ· 經濟部智慧財產局員工消費合作社印製 發明詳細說明： 請參閱第1圖。圖中所示為一晶圓處理系統範例，其 中包含一或多處理室12及14，該等處理室12,14位於一 共用工作區1 6中，該共用工作區1 6則為一牆1 8所圍繞。 處理室1 2及14得與一控制器22以資料相通，其中該控 器22與一或多監視器相接，如圖中24及26所示。一般 而言，監視器用以顯示處理室1 2，1 4相關製程的共用資 訊。監視器26之一位於牆18之上，另一監視器24則位 於工作區1 6内。對處理室1 2及14之操作控制得以一光 筆（光筆作用於監視器24,26之相對應一者）為之，即藉光 筆與控器溝通22達控之效。舉例而言，光筆28作用於監 第1〇頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X 297公釐） 567544 五、 經濟部智慧財產局員工消費合作社印製 發明説明（） 視器24 ’其得經由& 由皿視裔24與控器溝通；光 控制器28與控制器22溝通。 j丄由. 一 圖及第2圖。其中，處理室12及14之每 一者皆包含一機殼3〇、一茗 牛 側壁36，其中機殼 3 0 具有 底 离 7 Ο Jii- ^ Λ Λ /、底部牆32對立，側壁36 則位於機殼3 〇及芸Α 1 /々叫 及盖件34之間。機殼3〇構成一室37，一 座檯38位於處理它 至7中，用以支撐半導體晶圓等基材。 座檯38可受支撐而狡紅μ $从 動於盍件3 4及底部牆3 2之間，移 動者為-位移機構(未顯示）’但其位置一般為固定者。處 理氣體39a’39b及39c之供應器利用一蓮蓬頭與處理室η 以流體流動之方★、、甚，g 分· -本 式溝通，該二處理氣體39a，39b及39〇則 經流量閥41而受調節。 層膜沉積之前，基材得依所行之製程而為座檯38中 一加熱器加熱一所需溫度。舉例而言，座檯38可以阻性 方式加熱，其方式為自交流電源供應器43提供一電流加 …、零件44中。接著’基材42即為座檯38加熱，並可維 持在所需溫度範圍上，如約2〇它至約75 of間。一溫度感 測器46 (如一熱電偶）亦内嵌於晶圓支撐座檯38中，藉以 以傳統方式監視座檯3 8溫度。舉例而言，所測得溫度得 送入回授迴路中，藉以控制電源供應器43送至加熱零件 44中的電流，以使基採溫度得維持或控制於該製程的所需 溫度上。另外，座檯3 8亦可選擇性由轄射熱（未顯示）加 熱。此外，一真空幫浦48用以對處理室37抽氣，並用以 輔助維持正確氣流及處理室3 7内壓力。 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) (請先閱讀背面之注意事項再場寫本頁) # 567544 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明説明（） 請參閱第1圖及第2圖。圖中，兩處理室12及14之 一得利用後續沉積技術而於基材上沉積耐熱金屬層，其中 後續沉積技術之一異包含原子層沉積（ALD)技術。此處所 言之「基材」包含基材（如半導體基材及玻璃基材）及其上 方層膜（如介電層（即二氧化石夕））及阻障層（即鈦、氮化鈦 等）。 第3圖為一基村的剖面示意圖，其中顯示後續沉積時 一基材上一還原劑之可能吸附機制，其並未考慮及理論。 此處所言「吸附」一詞係包含化學吸附、物理吸附或任何 可工作及/或可提供一基材之一曝出表面之一部份上結 合、反應、黏著或佔據作用之吸引力及/或結合力。在本發 明之後續沉積技術進行當中，一第一處理氣體（在本例 為Aax)於基材42上形成一層，’A”，其中該基材42具有 配位基a表面，該配位基表面暴至處理室3 7環境；而” 層可為一單層、超過一單層或少於一單層。其後， 氣體進入處理室37成為清洗氣體”a心”，其尚未組合形 A層。第4圖為一基材之剖面示意圖，其中顯示還原劑 入後基材上方一含耐熱金屬化合物之可能吸附機制，當 洗氣體”Aax”從處理室37流出之後，一第二處理氣體，，Bb 導入處理室37中。基材表面上存在的”a”配位基與，，b，，配 基及’’B”原子作用而形成分子”ab”及”aa，，等，該等分子移 基材42處，並接著從處理室37中抽除。以此方式為之， 一包含一 B化合物層之表面仍留於基材42之上，並曝至 處理室37環境中，如第4圖所示。b化合物層的組 第12頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐） (請先閲讀背面之注意事項再填寫本頁) 中 A' 一清洗 成 導清 位 離 成可
567544 A7 B7 五、發明説明（） (請先閲讀背面之注意事項再填寫本頁) 為由 ALD技術形成之一單層或缺少原子之層。在其它實 施例中，每一次可形成之B化合物皆超過一單層。此外， 化合物B層得包含一多原子層（即B原子以外之原子）。此 時，第一及第二處理氣體得包含處理氣體之混合物，且該 兩處理氣體皆有原子與基材4 2黏附。該製程一次一次進 行，直至達到所需厚度。 請參閱第3圖及第4圖。處理氣體得為任意種類，在 本例中還原劑nAax”可至少包含B2H6或PH3 ;而含耐熱金 屬化合物則至少包含WF6。此時以下兩化學反應式（1)及（2) 所示為可能發生的反應： (1) B2H6(g) + WF6(g)---> W(s) + 2BF3(g) (2) PH3(g) + WF6(g) — — > W(s) + PH3(g) 〇 其它副產物包含（但非限定僅包含）氫、氫氟酸及氟。此外， 亦有其它反應發生的可能，如分解反應等。在其它實施例 中，其它還原劑亦得使用之，如SiH4等。同樣地，在其 它實施例中其它含挨氣體可適用之，如W(CO)6等。 經濟部智慧財產局員工消費合作社印製 清洗氣體包含氬、氫、氮、氦其它適用氣體及上述氣 體之混合物。清洗氣體可使用之種類可為一種或一種以 上。第5圖為使用兩種清洗氣體氬及氮時處理處理室中存 在氣體的一實施例，其中每一處理氣體皆由一載氣送入處 理室37中，在本例中該載氣為該等清洗氣體之一者，即 WF6為氬所送入，而B#6為氮氣所送入。不過，當了解 清洗氣體得與載氣為不同者，以下將有更詳細的介紹。本 發明中ALD技術進行的每一次皆包含於時間區間11内流 第13頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐） 經濟部智慧財產局員工消費合作社印製 567544 A7 五、發明説明（ 入氮清潔氣體至處理室3 7的步驟，复 ，、T時間@ 約〇·〇1至約15秒鐘，且為B2H6流至處理室幻°° a U歷時 時間區間t2時，處理氣體hi流 中別發生。 土 k理室3 7 φ 間歷時約〇 · 01秒至約15秒鐘，其中Β ή 、 ’ t2區 入，在本例中該載氣為氮。在約〇 6 乂載乳伴隨送 1秒至約工5 後’t3區間内Β2Η6停止流入，氮氣則續流動於另2里結束 秒至約15秒鐘區段内，用以清洗處理室中的—約〇·〇1 間區間t4時（其歷時約〇至約3〇秒鐘），产/ 2ΪΪ6。在時 抽氣，以移除全部或大部份的氣體。在處理^至37破加以 後，時間區間t5載氣氬通入，歷時約 至37抽氣之 冰朴 01秒至約15秒妒， 接者，在時間區間t5後的時間區間t6 ， 、里， 再與載氣氬一塊通入處理室37中，复由* ；； Wp6 甲時間區間屁。士 約0 · 0 1秒至約1 5秒鐘。當WF & i隹入忐 土寺 田Wh進入處理室37之 止後，氬氣流仍持續流入〇. 〇 1秒至1 5秒鐘 終 間t7内之動作。其後，處理室37被加以：氣此區 或大部份内部氣體抽離。接著，時間 ：所有 于間&間t8歷時約
30秒鐘，如此便完成後續沉積步驟 I 俩蜋。該循環之勒 作得持續進行，直至沉積之鎢膜達至所需厚度止 後續沉積技術之使用得有多重益處，复 、 /、甲包含層膜 形成與通量無關，故而沉積均勻度與基材大 、 土 小無關。例 例而言，由相同沉積室下一 200毫米基材及— 3 〇 〇亳乎 基材上所測得之層膜均勻度及厚度的差異是 ' " °』忽略的。 再者’該種技術能在複雜表面上得到較传的本 J罕乂住的步階覆蓋么士 果。 、° 第14頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X 297公釐） f請先閱讀背面之注意事項再填寫本頁}
567544 A7 B7 五、發明説明（） (請先閱讀背面之注意事項再填寫本頁) 此外，B層厚度（可參見第4圖）可輕易受到控制、並 同時使其阻抗達最小化，藉由後續沉積技術即可達成 之。請參閱第 6圖。由圖中線50之斜率可知，鎢層 B 厚度與形成其之循環次數成正比。不過，鎢層的阻抗相 對上與層膜厚度較無關，此可由第7圖之線5 2的斜率得 知。因此，只需藉由後續沉積技術，耐熱金屬層之厚度 即可輕易控成為通入處理室中處理氣體之循環次數的函 數，該厚度與阻抗間的關係並可忽略。 第8圖顯示以後續沉積技術於一基材上之層膜形成 速率與該基材溫度之關係，並可知沉積速率與基材42溫 度相關。由線5 4之斜率可知，基材42溫度的增加確增 加了鎢層B之沉積速率。此外，該圖式還指出基材上得 形成少一單層、少於一單層或多於一單層之鑛，端視基 材溫度而定。舉例說明之，在5 6部份，沉積速率在2 5 0 °C時約為2埃/循環次數；在58處，沉積速率在450°C時 為5埃/循環次數。不過，鎢層之阻抗確大致與沉積厚度 無關，此得由第9圖得知。因此，鎢層之沉積速率得控 制為溫度的函數，同時得與鎢層阻抗無關。當然，一般 都能希望耐熱金屬層之整體沉積形成時間。 經濟部智慧財產局員工消費合作社印製 為達該目的，耐熱金屬層之塊體沉積得併入沉積製 程中執行之。一般而言，耐熱金屬層在一般處理室中之 塊體沉積只發生於孕核層形成之後。更詳而言之，界本 範例而言，鎢層之孕核以上述後續沉積技術於處理室1 2 中形成，其中基材42加熱成約200°C至400°C，處理室 第15頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X 297公釐) 567544 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明説明（） 3 7則加壓成約1托爾至10托爾。於是，一孕核層6 0形 成於一經圖案化之基材42上，其厚度約120至約200 埃，如第1 0圖所示。結果更可發現，各種厚度之孕核層 皆得在對深寬比約6 : 1或更大之孔洞的填充時得到良好 的步階覆蓋結果，如約1 00埃或更小厚度者、約5 0埃或 更小厚度者、或約25埃或更小厚度者。由圖可知基材42 包含一阻障層61及一經圖案化之層，其中並有複數個孔 洞6 3，而孕核層係形成於覆蓋孔洞6 3之經圖案化層旁。 由結果可知，利用ALD技術形成之孕核層60得有良好 步階覆蓋結果。在另一實施例中，後續沉積技術可用於 孕核及塊材的沉積上。在另一實施例中，鎢層之全部沉 積時間得以降低，其係以CVD法進行鎢塊材於孕核層60 上的沉積、同時基材42係置於第1圖所示之同一沉積室 1 2上。塊材之沉積得以習用參數及方法進行，如此得行 完整插塞填充之鎢層6 5得形成於經圖案化之層膜上，其 中填充之孔洞的深寬比約為6: 1，如第1 1圖所示。 在另一不同實施例中，一分叉沉積製程得使用之， 其中耐熱金屬層的孕核係發生於其它耐熱金屬層部份形 成之不同處理室中。更詳而言之，本範例中的鎮層孕核 係利用後續沉積技術（如上述之ALD)使發生在處理室12 中，此時得使基材42加熱成約200 °C至約400 °C、並使 加壓成約1托爾至約1 0托爾間之方式為之。 在一實施例中，後續沉積技術用於處理室1 4中置有 基材42(如第1圖所示）、且該基材42進行孕核層60上 第16頁 (請先閱讀背面之注意事項再填寫本頁) ,裝· 、可· # 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) 567544 A7 B7 五、發明説明（） 塊體沉積時，其中塊體沉積得以本文所揭露之參數為 之。在另一實施例中，上述塊體沉積則係以CVD技術為 之，其中的沉積參數得以該項技術所慣用者為之。不論 所用方式為後續沉積或CVD技術，所得鎢層65皆得在 具深寬比約6 : 1之孔洞的具圖案化層膜上達成完整的充 塞填充效果，如第1 1圖所示。藉執行上述之分叉沉積製 程，較佳特性鎢層的形成時間得以降低，CVD塊體沉積 的使用則能更增產率。 如上所述，本發明一不同實施例之載氣得與清洗氣 體為不同者，如第1.2圖所示。其中，清洗氣體至少包含 氬，並分別在時間區間tl、t3、t5及t7間導入；載氣則 至少包含氮，並在時間區間t2及t6導入。故而，時間 區間t2時，導入處理室之氣體包含B2H6及N2 ;時間區 間t6時，導入者則包含WF6及N2。時間區間t4及t8 時，所用之抽氣方式與第5所述者同。在又另一實施例 中，時間區間t2及t6内的載氣至少包含氫，而此時於 時間區間tl、t3、t5及t7内導入之清洗氣體至少包含氬。 時間區間t4及t8時，抽氣處理與上述者同。故而，時 間區間t2時，通入處理室37之氣體混合物至少包含B2H6 及氫；時間區間t6時，所導入者則至少包含WF6及氫。 以氫為載氣具有提升鎢層B穩定度的效果。更詳而 言之，孕核層60内之氟濃度（如第10圖所示）在以氫為 載氣時顯得相當低，此係與以氮化氬為載氣之時的比 較。 第17頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) (請先閲讀背面之注意事項再填寫本頁) 、τ #· 經濟部智慧財產局員工消費合作社印製 567544 A7 B7 五、發明説明（） 請參閱第14圖及第15圖。圖中，曲線66之高點與 低點說明氟濃度可超過1 X 1 021個原子/立方公分，最低則 仍有1 X 1 0 1 9個原子/立方公分；但在曲線6 8中，氟濃度 之高點確低於1 X I 021個原子/立方公分，而其低點顯示氟 濃度確低於1 X 1 〇 17個原子/立方公分。因此，以氫為載氣 確能提供遠較穩定之膜層，即氟擴散至基材或相鄰層之 機率得以降低。此外，因氟濃度增加而生成的金屬氟化 物得以避免之，故耐熱金屬層之阻抗亦得因此降低。故 而，孕核層之穩定度及其阻抗得控制成所用載氣之函 數。當沉積係全以ALD技術為之時（即不使用其它C VD 等技術），該事實亦適用於此處。 此外，若在含鎢化合物通入前吸附PH3或B2H6層（如 第1 6圖所示），所形成之鎢層72得具有較低之氟含量、 較佳之步階覆蓋結果及較佳之阻抗，此項事實可由含鎢 化合物利用後續沉積或標準CVD沉積、並以WF6及SiH4 或WF6及氫氣形成於PH3或B2H6層時獲得印證。此鎢 膜所獲得的較佳特性相信是因PH3或B2H6層及WF6層 間的化學親合性所致，此親合性得提升被吸附化學物質 之表面移動性及有效降低鎢膜於孕核階段之 WF6。此 外，此項特性還被證實有助於鎢層沉積於含鈦黏著層（由 鈦或氮化鈦形成者）之旁。層膜7 0以為一單層為佳，但 在其它實施例中可為少或多於一單層；由第16圖之膜層 堆疊中的層膜70得知鎢層72的形成。可以了解的是， 層膜70可或不可於鎢層72形成之時消耗，複數層70及 第18頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐） (請先閱讀背面之注意事項再填寫本頁) 句· # 經濟部智慧財產局員工消費合作社印製 567544 A7 B7 五、發明説明（） (請先閲讀背面之注意事項再填寫本頁) 鎢層72可利用沉積而將鎢層形成至一所需厚度。由圖可 知，層膜7 0沉積處之基材7 4包含任何得為半導體處理 材料所形成之晶圓7 6，如矽等；晶圓7 6上可形成之層 膜可為一或多者，如圖中之層膜74;層膜78得為任何 適用材料所形成，包含介電或導電材料，其中層膜78包 含一孔洞8 0，用以暴出晶圓7 6之一區域8 2。 第1 8圖為一基材之詳細剖面圖，其中一含鈦黏著層 形成於一基材及一 Ρ Η 3或B 2 Η 6層間，此係用以在含鈦黏 著層相鄰處形成一鎮層。用在一實施例中，該含鈦黏層 的形成係以後續沉積技術為之，且處理氣體 Aax為自 氫、B2H6、SiH4及NH3組成之群組中選出者，而鈦氣體 則係選自TDMAT、TDEAT及TiCl4所組成的群組中者。 此外，氬及氮清洗氣體亦相對較為適用，不過其它清洗 氣體亦可使用之。 經濟部智慧財產局員工消費合作社印製 請參閱第2圖及第17圖。其中，每一處理氣體都伴 以一載氣送入處理室3 7中，在本範例中該載氣為該等清 洗氣體之一者。不過，當了解的是清洗氣體得不同於載 器，以下將有更完整的說明。本發明中，後續沉積技術 的一循環包含在含鈦氣體流入處理室3 7前、送入一清洗 氣體至處理室中（時間區間11) ^之後，該含鈦處理氣體 被送入處理室3 7中（時間區間t2)。接著，含鈦氣體停止 送入，載氣則持續通入以清洗處理室中的含鈦處理氣體 (時間區間t3)。時間區間t4時，對處理室37抽氣，以 使所有氣體皆移出。處理室3 7經抽氣後，一載氣在時間 第19頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X 297公釐) 567544 A7 B7 五、發明説明（） (請先閱讀背面之注意事項再填寫本頁) 區間t5時通入。接著，還原處理氣體由載氣伴隨通入處 理室37中（時間區間t6)。流進處理室37之還原處理氣 體流接著停止，但載氣的流入動作仍持續（時間區間 t7)。其後，處理室3 7被抽氣，以將内部所有氣體移除（時 間區間18 )，如此驗完成本發明之後續沉積技術的一整個 循環。為使含鈦層達到其所需厚度，上述循環必須不斷 執行（至所需厚度達成為止）。舉例而言，在氮化鈦層8 4 達成所需後度之後，層膜86(在本範例中係以PH3或B2H6 形成者）便以後續沉積技術形成於其旁（可參閱第 18 圖），如上所述者。其後，一鎢層8 8以後續沉積技術或 標準CVD技術形成於該層86之旁，其中該兩項沉積技 術的進行皆已詳述如前。層膜8 6以為一單層為佳，但在 其它實施例中可為多於或少於一單層。在第18圖中，層 膜堆疊中之層膜86顯示鎢層88的形成，其可在鎢層88 形成時消耗或不消耗，且複數層膜8 6及鎢層6 6得沉積 形成一所需厚度之鎢層。若有沉積金屬銅之必要，此時 銅膜得沉積於該鎢層8 8之上，此時鎢可當作之銅之阻障 層。 經濟部智慧財產局員工消費合作社印製 請再參閱第2圖，其中說明鎢層之沉積製程得以一 電腦程式產品控制，該電腦程式產品為控制器 22所執 行。為達以控制器2 2執行之目的，控制器中包含一中央 處理單元（CPU)90、一揮發性記憶體（如隨機存取記憶體） 及永久儲存媒體（如磁碟片所用之軟碟裝置、或硬碟裝置 94)。電腦程式碼可以各種傳統電腦可讀取程式語言寫 第20頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) 567544 A7 B7 五 經濟部智慧財產局員工消費合作社印製 發明説明（） 入’如 68000 組合語言、C、C + +、Pascal、Fortran 等。 既撰成之適用程式碼輸進一單一或多個樓案中，即利用 傳統文字編輯器撰成而存於一電腦可讀取媒體中，如硬 碟裝置中。若所輸入的碼文字屬於高階語言，該程式需 先經過編譯，所得到的編譯碼再與W i n d 〇 w s庫常式預先 編澤完成之物件碼連結。當欲執行該經連結及編譯之物 件碼時，系統使用者先喚起物件碼，以使CPU 90將 式竭載進RAM 92，再由CPU 90讀取及執行該程式瑪 藉以執行程式中指定將執行的任務。 以上已利用各實施例進行本發明之說明，然熟習 項技術者仍得對其中的反應條件（即溫度、壓力、膜層 度等）加以改變，此類變更仍屬本發明之範圍。此外， 述說明指出分叉沉積製程係於同一系統中進行，但塊 沉積得於孕核層形成之處理室所在之主沉積系統以外 主沉積系統處理室中進行。最後，所得沉積者除可為 以外’其它耐熱金屬亦得藉由本發明之方式加以沉積 且CVD沉積法得以其它沉積技術代替之。舉例而言， 理氣相沉積（PVD)或CVD與PVD之聯合使用皆為可 者。是以，本發明之範圍不應以上述說明界定，而各 後附包含所有本發明等效者之申請專利範圍所戴者為實 際範圍。 第21頁 程 (請先閱讀背面之注意事項再填寫本頁) 該 厚 上 體 的 嫣 物 行 以 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐）

Claims (1)

  1. 567544
    經濟部智慧財產局員工消費合作社印製 A8 B8 C8 D8 申請專利範圍 1. 一種對一處理室中一基材上一鎢孕核層進行後續沉積 之方法，其至少包含下列步驟： 導入一還原劑，該還原劑係自PH3及B2H6所組成 之群組中選出者；及 導入一含鎢化合物。 2 ·如申請專利範圍第1項所述之方法，其中該孕核層形 成於一含鈦層上。 3 ·如申請專利範圍第1項所述之方法，其中一鎢塊材層 係形成於該孕核層上。 4 ·如申請專利範圍第3項所述之方法，其中該鎢塊材層 係由後續沉積方式形成。 5 ·如申請專利範圍第3項所述之方法，其中該鎢塊材係 由化學氣相沉積法形成。 6.如申請專利範圍第3項所述之方法，其中該嫣塊材係 由物理氣相沉積法形成。 7 ·如申請專利範圍第3項所述之方法，其中該孕核層及 該鎢塊材層的形成係在同一處理室中完成者。 第22頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) (請先閱讀背面之注意事項再填寫本頁) 567544 A B CD 六 經濟部智慧財產局員工消費合作社印製 申請專利範圍 8. 如申請專利範圍第3項所述之方法，其中該孕核層及 該鎢塊材能係於不同處理室中形成者。 • ί 9. 如申請專利範圍第2:續所述之方法，其中該含鈦層及 該孕核層係於不同處理室中形成者。 10. —種在一處理室中一基材上沉積以一鎢層之方法，其 至少包含下列步驟：： 吸附一層膜於該基材之上，該層膜至少包含由ΡΗ3 及Β 2 Η 6組成之群組中選出之一化合物；及 導入一含鎢化合物，以形成一鎢層。 1 1 .如申請專利範圍第1 0項所述之方法，其中該導入一 含鎢話合物之步驟至少包含在一後續沉積處理中導入 一含鶴化合物的步驟。 1 2 .如申請專利範圍第1 0項所述之方法，其中該導入一 含鎢化合物之步驟至少包含於一化學氣相沉積處理中 導入一含鎢化合物之步驟。 1 3 .如申請專利範圍第1 0項所述之方法，其中該吸附層 形成於一含鈦層之上。 14.如申請專利範圍第10項所述之方法，其中該吸附一 第23頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X 297公釐) (請先閲讀背面之注意事項再填寫本頁) 567544 ABCD 六 經濟部智慧財產局員工消費合作社印製 申請專利範圍 層膜及導入一含鎢化合物之步驟係於同一處理室中進 行。 1 5 .如申請專利範圍第1 0項所述之方法，其中該吸附一 層膜及導入一含鎢化合物的步驟係於不同處理室中進 行。 1 6. —種處理一基材之處理系統，其至少包含： 一本體，構成一處理室； 一固定支撐器，位於該處理室之内，用以支撐該基 # ; 一氣體傳送系統，以流體流動之方式與該處理室相 通；及 一控制器，在電性上與該氣體傳送系統相通； 一記憶體，與該控器以資料相通，該記憶體至少包 含一電腦可讀取媒體，該電腦可讀取媒體中具有一電 腦可讀取程式，該電腦可讀取程式包含一組指令還原 劑導入指令及含鎢化合物導入指令，用以形成一孕核 層，其中該原原劑係自ph3及B2H6組成之群組選出 者。 1 7.如申請專利範圍第1 6項所述之處理系統，其中該電 腦可讀取程式包含一第二阻指令，用以在該孕核層上 形成一嫣塊材層。 第24頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐) (請先閲讀背面之注意事項再填寫本頁)‘ 567544 8 8 8 8 A B CD 六、申請專利範圍 1 8 ·如申請專利範圍第1 6項所述之處理系統，其中更包 含： 一第二本體，構成一第二處理室； 其中該控制器在電性上與該第二本體相通；及 其中該第二組指令控制該鎢塊材層於該第二本體 中的形成。 (請先閲讀背面之注意事項再填寫本頁) 裝· 經濟部智慧財產局員工消費合作社印製 第25頁 本紙張尺度適用中國國家標準(CNS)A4規格(210X297公釐)
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US7749815B2 (en) 2010-07-06
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WO2003009360A2 (en) 2003-01-30
WO2003009360B1 (en) 2003-12-04
US6936538B2 (en) 2005-08-30
US7238552B2 (en) 2007-07-03
US20080014724A1 (en) 2008-01-17
US20030013300A1 (en) 2003-01-16
JP4705325B2 (ja) 2011-06-22
WO2003009360A3 (en) 2003-10-30

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