TW567584B - Process for producing oxide thin films - Google Patents

Process for producing oxide thin films Download PDF

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Publication number
TW567584B
TW567584B TW090108955A TW90108955A TW567584B TW 567584 B TW567584 B TW 567584B TW 090108955 A TW090108955 A TW 090108955A TW 90108955 A TW90108955 A TW 90108955A TW 567584 B TW567584 B TW 567584B
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source material
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film
pulse
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TW090108955A
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Matti Putkonen
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Asm Microchemistry Oy
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    • H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
    • H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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    • 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
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    • C23C16/45531—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 ternary or higher compositions
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  • Formation Of Insulating Films (AREA)

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567584 A7 B7 五、發明説明（1 ) 發明領域 ' (請先閱讀背面之注意事項再填寫本頁) 本發明有關一種藉A L D方法製造之氧化物薄膜。本 發明尤其有關一種經釔安定化之氧化鉻（γ s Z )薄膜。 相關技藝描述 微電子組件不斷地縮小導致目前使用於金屬氧化物半 導體場效電晶體（Μ〇S F E T )中作爲閘極氧化物之 S i〇2需使用較高電容率氧化物取代。此因爲了達成所需 之電容，該S i〇2層應製得較薄，故穿隧電流會增加到影 響組件功能的程度。此種問題可使用介電常數高於S i〇2 之介電材料得到解決。例如，動態隨機存取記憶體（ D R A Μ )電容器之電容需在尺寸迅速縮小的同時保持接 近常數，因此需使用電容率高於此等材料且產生較高電容 密度之材料取代先前使用之S 1〇2及S i 3 Ν 4。 經濟部智慧財產局員工消費合作社印製 有數種具有充分高之介電常數的材料，但除了高電容 率以外，此等介電薄膜需特別具有低漏流密度及高介體破 壞電場。此等性質中同時達到兩項之前提係爲致密且無缺 陷之薄膜結構。亦重要的是該材料穩定地與矽接觸，且可 曝露於高處理高溫下，而基本上不變。尤其是閘極氧化物 之應用中，重要的是在介於矽與具有高介電常數之金屬氧 化物之間的界面中，具有極少之電活性狀態。記憶體應用 中，重要的是該電容器之介電體結構穩定，因爲用以活化 植入離子之溫度極高。 氧化鉻Z r 0 2係爲具有高熔點及良好化學安定性之絕 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -4 - 567584 經濟部智慧財產局員工消費合作社印製 A7 B7 五、發明説明（2 ) 緣材料。Z r 0 2可藉著添加其他氧化物而進一步安定化， 添加其他氧化物之目的係消除Z r 0 2之相變化。一般，該 單斜晶形式係穩定至1 1 0 0 °C，而四方晶到2 2 8 5 °C ，再高就屬立方晶系爲穩定狀態。穩定化一般係藉添加氧 化釔（Y 2〇3 )而進行，但亦可使用M g〇、C a〇、 Ce〇2、1112〇3、0(12〇3及厶12〇3。以往係製造 Y S Z薄膜，例如使用金屬-有機化學氣相沉積（ Μ 0 C V D ) ( Garcia, G·等人 Preparation of YSZ layers by MOCVD: Influence of experimental parameters on the morphology of the film, J. Crystal Growth 1 56 ( 1 995), 426 )及 e —束蒸發技術（比較 Matth6e，Th. et al·，Orientation relationships of epitaxial oxide buffer layers on silicon ( 100) for high-temperature superconducting YBa2Cu3〇?-x films，Appl. Phys. Lett. 6 1 ( 1 992)，1 240 )製得。 原子層沉積（A L D )可用以製造二元氧化物薄膜。 ALD - —原來稱爲原子層磊晶（ALE) —一係爲習用 CVD之變化方式。該方法名稱最近由AL E變成ALD ，以避免在討論多晶形及非晶形薄膜時產生混淆。使用於 A L D 之設備係爲 ASM Microchemistry 〇y, Espoo，Finland 所製商標A L C V D τ M者。該A L D方法係基於連續之自 身飽和化表面反應。該方法係詳述於美國專利第 4， 0 5 8, 43〇號及第5， 711， 811號中。使 用惰性載體及淸洗氣體之長晶優點係使該系統更爲快速。 使用A L D式方法製造較複雜之複合物時，所有組件 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公慶） ^_ (請先閱讀背面之注意事項再填寫本頁) 訂 -5- 567584 A 7 B7 五、發明説明（3 ) (請先閱讀背面之注意事項再填寫本頁) 皆無法在相同反應溫度範圍內具有一個用以控制長晶之 ALD程序限幅。Μδΐ sS等人發現ALD式長晶可在生 長二元組份時得到，即使未發現真實之A L D限幅亦然， 但該薄膜之長晶速率係視溫度而定（M01s3，H.等人，Adv. Mat. 〇pt. Ei. 4 ( 1 994)，3 8 9 )。使用此種來源材料及反應 溫度以製造固體溶液及經摻雜薄膜時，在需要準確之濃度 控制時發現困難。而且若小値溫度變化對於長晶方法具有 影響，則該方法變得更難以放大。 Μ δ 1 s 3 寺人（Μ ό 1 s S，Η ·等人，A d v · M a t.〇 p t · E1. 4 (1994)，389 )揭示一種藉ALE方法生長Y2〇3之方法。 其使用 Y(thd)3(thd = 2, 2， 6， 6 —四甲基 一 3， 5 -庚烷二酮）作爲釔源材料且使用臭氧一氧混合 物作爲氧源材料，溫度範圍4 〇 〇 一 5 〇 〇 t。如前文所— 述，未發現A L E限幅，因爲長晶速率穩定地隨著溫度增 高而自0 · 3埃/周期增加至1 · 8埃/周期。
Ritala 等人（Rhala，M.及1^1^〇13，以.，八？？1.3訂[
Sci. 75 (1994)，333 )揭示一種藉A LD式方法生長 經濟部智慧財產局員工消費合作社印製 Z r〇2之方法。Z r C 1 4係作爲鉻源材料，而水係作爲 氧源材料。該程序中之溫度係爲5 〇 〇 °C，而長晶速率係 爲0 · 5 3埃/周期。 發明槪要 本發明之目的係解決先前技藝之問題，且提出一種新 穎之製造經釔安定化之氧化鉻（Y S Z )薄膜的方法。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -6- 567584 Α7 Β7 五、發明説明（4 ) 此項及其他目的與其優點係藉著下文描述及申請之本 發明達成。 (請先閲讀背面之注意事項再填寫本頁) 本發明係基於氧化釔及氧化鉻可藉著A L D式方法長 晶之發現，故該薄膜生長係依據A L D原理，而形成經釔 安定化之氧化锆薄膜。 詳言之，用以製造YSZ薄膜之方法之特徵爲申請專 利範圍第1項之特徵部分所陳述者。 使用本發明達成數項重要之優點。 經§乙女疋化之氧化錯薄膜的長晶速率局，例如， A L D薄膜之長晶速率約較基於Z r〇2及Y 2〇3之長晶 速率預測者高約2 5百分比。 使用於本發明之溫度較先前技藝方法低，降低製造方 法之成本。 本發明方法之薄膜生長具有良好之薄膜性質。因此， 所得之氧化物薄膜即使在不均勻表面上，仍具有優越之服 貼性。該方法亦對薄膜生長提供優越且自動之自身控制性 〇 經濟部智慧財產局員工消費合作社印製 經A L D生長而經釔安定化之氧化鉻薄膜可作爲例如 電子零件及光學零件中之絕緣體。例如，於場致發光顯示 器（F E D )中，以使用具有光滑表面之絕緣氧化物爲佳 。使用Y S Z薄膜作爲氣體感測器及燃料電池中之固體電 解質亦佳。尤其適於使用Y S Z薄膜作爲微電子裝置中之 閘極氧化物，且作爲動態隨機存取記憶體（D R A Μ )中 之電容器。 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ 297公釐） 567584 A7 B7 五、發明説明（5 ) 其次，針對以下詳述且參照附圖詳細地描述本發明。 圖式簡單說明 (請先閱讀背面之注意事項再填寫本頁) 圖1以長晶溫度之函數表示Y 2〇3之長晶速率。 圖2以來源材料之脈衝時間之函數表示Y 2〇3之長晶 速率。 圖3以反應周期數之函數表示Y 2 0 3薄膜之毫微米厚 度。 ，： 圖4以長晶溫度之函數表示Z r〇2 g表晶速率。 圖5以脈衝時間之函數表示Z r〇2之長晶速率。 圖6以反應周期數之函數表示Z r〇2薄膜之厚度。 圖7表示於3 0 0°C及4 5 Ot下生長之Z r〇2薄膜 的X —射線繞射（X r D )圖型。 圖8表示Z r〇2、¥32及¥2〇3薄膜之脈衝順序 〇 圖9以薄膜中之Y2〇3含量之函數表示γ S Z薄膜之 長晶速率。 經濟部智慧財產局員工消費合作社印製 圖1 0表示於（1 00)矽基材上生長之YSZ薄膜 (厚度9 0毫微米）之XRD圖型。 圖1 1以Υ2〇3濃度之函數表示YSZ薄膜之XRD 圖型中（2 0 〇)平面之之d -値（平面間隔）變化。 圖1 2以Y2〇3濃度之函數表示YS Z薄膜中之氯濃 度。 圖13表示（1〇〇)矽基材（a) 、YSZ薄膜（ 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -8 - 567584 A7 B7 五、發明説明（6 ) 10重量百分比之Y20 3，厚度120毫微米，！3)之 1 R〜光譜及扣除後之光譜（c ) 〇 (請先閱讀背面之注意事項再填寫本頁) 圖1 4表不Y2〇3濃度於中〜I R —區中的波數相依 性。 圖1 5表示使用不同分析方法測量之Y / Z r比例。 發明詳述 疋我 本發明中，” A L D式方法”意指其中材料自氣相或 蒸發來源化學品長晶於表面上之過程，係基於依序及交替 之自身飽和化表面反應之方法。A L D之原理係揭示於例 如 US 4 0 5 8 43〇及 5 711 811 中。 ”反應空間”用以表示其中條件可調整，以藉ALD -長晶之反應器或反應槽。 ” A L D限幅”用以表示根據A L D原理生長薄膜之 溫度範圍。根據A L D原理生長薄膜之一表示，係該長晶 速率於該溫度範圍內基本上保持定値。 經濟部智慧財產局員工消費合作社印製 ”薄膜”用以表示經由真空、氣相或液相，以個別離 子、原子或分子形式，自該來源傳送至該基材之元素或化 合物所生長之薄膜。該薄膜之厚度係視應用而定，大幅變 化，例如，由一分子層變成8 0 0毫微米，或最多達1微 米，或甚至更厚。 ^ 長晶方法 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -9- 567584 A7 B7 五、發明説明（7 ) 根據本發明，該氧化物薄膜係藉A L D方法製得。因 此，反應槽中所放置之基材係進行至少兩種氣相試劑之依 序、交替重複表面反應，以於其上層生長薄膜。 (請先閱讀背面之注意事項再填寫本頁) 反應空間中之條件經調整，使得不發生氣相反應，即 氣體試劑之間的反應，而僅發生表面反應，即吸附於基材 表面上之物質與氣體試劑之間的反應。因此，氧來源材料 分子與吸附於表面上之金屬來源化合物層進行反應。此種 長晶係依循A L D原理。 根據本發明方法，該金屬來源材料與該氧來源材料之 氣相脈衝係交替且依序地進料至該反應空間中，而與裝置 於該反應空間內的基材表面接觸。該基材之，，表面”原始 上包括實際基材之表面，其視情況預先經處理，例如，與 化學物質接觸，以修飾其表面性質。在該薄膜長晶過程中— ，先前金屬氧化物層形成表面，以供後續金屬氧化物層使 用。該試劑較佳係借助惰性陽離子性氣體諸如氮進料至該 反應器中。 經濟部智慧財產局Μ工消費合作社印製 較佳且使該方法較佳之方式係該金屬來源脈衝及氧來 源材料脈衝係藉惰性氣體脈衝彼此分離，亦稱爲氣體沖洗 ，以沖除反應空間中先前化學物質未反應之殘留物及反應 產物。該惰性氣體沖洗一般包括非活性氣體，諸如氮，或 局貴氣體諸如氬。 因此，一脈衝施加序列（亦稱爲”周期”或”反應周 期”）較佳係包括以下步驟 -借助惰性氣體將金屬來源化學物質之氣相脈衝進料 财關家縣（⑽）Μ規格（210X297公釐) -10- 567584 A7 B7 五、發明説明（8 ) 至該反應空間內； -使用惰性氣體沖洗該反應空間； . (請先閱讀背面之注意事項再填寫本頁) 將氧來源材料之氣相脈衝進料至該反應空間內；及 -使用惰性氣體沖洗該反應空間。 該沖洗時間係選擇長至足以防止氣相反應，且防止金 屬氧化物薄膜生長速率高於該氧化物每個周期之最佳 A L D生長速率。 該沉積可於常壓下進行，但較佳係於減壓下操作該方 法。反應器中之壓力一般係爲〇·〇1—20毫巴，以 〇.1 一 5毫巴爲佳。 該基材溫度需低至足以保持薄膜原子間之鍵結緊密， 而防止氣體或蒸發試劑之熱分解。另一方面，該基材溫度 需高至足以使來源材料保持於氣相，即需避免該氣體或蒸、-發試劑冷凝。此外，該溫度需高至足以提供表面反應之活 化能。於基材上生長氧化锆時，基材溫度一般係2 5 0 -5〇〇°C，以275 — 45〇°C爲佳，尤其是275 — 經濟部智慧財產局員工消費合作社印製 3 2 5 °C。用以於基材上生長Y 2〇3之溫度範圍一般係爲 2〇〇一 4〇〇°C,以250 — 35〇°C爲佳。該YSZ 薄膜一般係於25〇一 400 °C生長，以275 — 35〇 °C爲佳，尤其是275 — 325 t：。 _ 此等情況下，鍵結於該表面上之試劑的量係由該表面 決定。此種現象稱爲”自身飽和化”。基材表面上之最大’ 覆蓋性係於吸附單層金屬來源化學分子時得到。重複施加 脈衝之序列，直至生長了具有預定厚度之氧化物薄膜。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -11 - 567584 Μ Β7_ 五、發明説明（9 ) (請先閲讀背面之注意事項再填寫本頁) 來源溫<度較佳係設定於低於基材溫度。係此基於若來 源化學蒸汽之分壓超過基材溫度下之冷凝極限，則喪失該 薄膜受控地逐層生長之事實。 自身飽和化反應之時間量大多由經濟因素諸如來自反 應器之產物通量所限制。使用相對少之施加脈衝周期製得 極薄之薄膜，某些情況下，此可增加來源化學脈衝時間， 因此，採用蒸汽壓低於一般物質之來源化學物質。 該基材可有各式各樣之種類，例如片形或粉狀。實例 包括矽、二氧化矽、經塗佈之矽、銅金屬、及各種氮化物 ，諸如金屬氮化物。 根據本發明生長之Y S Z薄膜一般係經（1 〇 〇 )定 向。 經濟部智慧財產局員工消費合作社印製 當來源材料中之一或多種含有氯時，包含锆及/或釔-之薄膜中會發現氯殘留物。本發明所製得之Y s Z薄膜中 ，該薄膜中C1濃度一般係爲〇.05-0.25重量百 分比。意外地發現就本發明而言，當所形成之薄膜中的釔 濃度低時，即低於2 0重量百分比時，尤其是低於1 5重 量百分比時，所形成之薄膜的氯含量係低於基本上由 Z r〇2所構成之薄膜。 、 前述脈衝施加序列中，金屬來源化學物質或爲鉻來源 材料或爲釔來源材料。因此，本發明長晶方法中，氧化釔 及氧化鉻係生長於基材上。 · 根據本發明較佳具體實例，形成經釔安定化之氧化鉻 薄膜。因此，在該薄膜生長期間，至少一個前述施加脈衝 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -12- 567584 A7 B7 五、發明説明（1〇) (請先閱讀背面之注意事項再填寫本頁) 周期係使用釔來源化學物質作爲金屬來源化學物質而進行 ，而至少一個前述施加脈衝周期係使用銷來源化學物質作 爲金屬來源化學物質進行。 釔來源化學物質及鉻來源化學物質之間的脈衝施加比 可經選擇，以得到薄膜所需之性質。一般，脈衝施加比Y :Z r係由1 : 1 0至1 〇 ·· 1，以1 : 5至5 ·· 1爲佳 ，而1 : 3至3 : 1更佳，脈衝施加比約1 : 1最佳。 圖8出示用以生長Z r〇2、YS Z及Y2〇3薄膜之 脈衝施加序列。圖8 ( b )中，說明Y S Ζ薄膜脈衝施加 比Y : Z r = 1 : 2時之脈衝施加序列。 圖9表示Y S Z薄膜之長晶速率，與針對個別氧化物 計算之値比較，以薄膜中Y 2〇3重量百分比之函數表示。 Y S Z長晶速率進行比較之値係藉著於各個脈衝施加比 Y2〇3 : Z r〇3下一起添加Y2〇3及Z r〇2之長晶速 率而計算，而此計算値於圖中係以1 〇 〇百分比表示。因 此，該圖顯示Y 2〇3 : Z r〇2脈衝施加比對於長晶速率 及Y S Z薄膜之釔濃度的影響。 經濟部智慧財產局員工消費合作社印製 根據本發明之一具體實例，第一脈衝施加周期中於基 材上生長Y S Z薄膜係使用釔來源化學物質作爲金屬來源 化學物質。 根據本發明另一具體實例，第一脈衝施加周期中於基 材上生長Y S Z薄膜係使用鉻來源材料作爲金屬來源化學 物質進行。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -13- 567584 A7 B7 五、發明説明（11) 來源材料 ' 釔及鉻之氣體或揮發性化合物係於本發明方法中作爲 金屬來源材料。 (請先閱讀背面之注意事項再填寫本頁) 因爲各金屬化合物之性質變動，故需考慮使用於本發 明方法中之各金屬化合物的適用性。該化合物之性質請參 照例如 Ν· N. Greenwood and A. Earnshaw，Chemistry of _Elements, 2nd edition, Pergamon Press，1997。 該金屬來源材料需選擇，以滿足充分蒸汽壓、於基材 溫度下之充分熱安定性及化合物之充分反應性的要求。 充分之蒸汽壓意指接近基材表面之處的氣相中，需有 足夠之來源化學物質分子，以於表面上進行快速充分之自 身飽和化反應。 實際上，充分熱安定性意指該來源化學物質本身必需-不會於該基材上形成擾亂長晶之可冷凝相，或經由熱分解 而於基材表面上留下有害程度之雜質。因此，一目標係避 免基材上無法控制之分子冷凝。 其他選擇標準包括高純度化學物質之可用性，及操作 簡易度、合理之預防措施。 經濟部智慧財產局員工消費合作社印製 此外，需考慮由配體交換反應所產生之副產物的&胃 。重要的是該反應產物基本上係爲氣體。意指該配體交換. 反應中可能形成之副產物係氣體，足以借助惰性氣體自@ 應空間移除，意指其不會在薄膜中成爲雜質。 1 .釔來源材料 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐） -14- 567584 A7 __B7 五、發明説明（12) ί乙來源材料一般係選自具有通式（I )或（Π )之材 料： (請先閱讀背面之注意事項再填寫本頁) Υ X 3 ( I ) γ X 3 Β ( Π ) 其中 X係選自下列者之群： 1 )具有通式（m)而自氧配位之二酮（即/3 —二酮 酸酯） 'r，Vyr’ 0 0 (III) 其中 R >及R 〃一般係相同，選自例如直鏈或分枝鏈C i 一 -Cl。^!；基，尤其是直鍵或分枝鍵Cl 一 C6院基，最佳係爲 ~ c Η 3 > - C (CH3) 3、— CF3 及—C ( C F 3 ) 3 ϋ )環戊二烯基， iii )具有式（W )之環戊二烯基衍生物： 經濟部智慧財產局員工消費合作社印製 C 5 Η 5 - y R m y ( IV ) 其中 R…選自例如直鏈或分枝鏈C i 一 C i 〇烷基，以C i 一 C6烷基爲佳，尤其是甲基（—CH3)、乙基、丙基、丁 基、戊基、及具有長碳鏈之院基、院氧基、芳基、胺基、 氰基及甲矽烷基，且 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -15- 567584 A7 ___ B7 五、發明説明（13) y係爲整數1一5，且 (請先閲讀背面之注意事項再填寫本頁) B係爲中性加合配體，其鍵結於來自一或多個原子之 中心原子。一般B係爲烴、含氧之烴（諸如醚）、含氮之 烴（諸如聯吡啶、二氮雜菲、胺或多胺）。 根據本發明之一具體實例，使用Y ( c 〇 t ) C p Μ c o t =環辛四烯基且c ρ* =五甲基環戊二烯基）作爲釔 來源材料。 根據本發明較佳具體實例，使用Y ( t h d )3 ( t h d 二2， 2， 6， 6 —四甲基一 3， 5 —庚烷二酮）作爲釔 來源材料。 2 ·錯來源材料 鉻來源材料一般係選自鉻鹵化物及包含至少一個碳原-子之銷化合物。 該鉻來源材料一般係選自具有通式（V )者 R 2 Z r X 2 ( V ) 其中 經濟部智慧財產局員工消費合作社印製 基 烯 二 戊 環 自 選。 係物 R 生 11—? 行 之 Η 式 通 有 具 其 及
IV
)2 _ ρ η C ， I 基 Α 烷 I 之 p a c 2 -Η (c 連c 橋式 況通 情有 視具 係 、 R 基 體甲 配爲 係 A 中 其 如 、 諸 r 烴：B 之群、 代之1 取體 C 經配、 或下 F 佳自基 爲選鹵 3 係 } 或 X i 2 以 Η 本紙張尺度適用中國國家標準（CNS ) A4規格（21GX297公釐） -16- 567584 A7 ______B7_ 五、發明説明（14) ϋ)氫（ — H)、直鏈或分枝鏈Cl 一 Cio院基，以 Cl—C6院基爲佳，尤其是甲基（―CH3)、乙基、丙 基、丁基或較長之烴鏈， (請先閲讀背面之注意事項再填寫本頁) 迅）甲氧基（一 OCH3)或其他直鏈（例如 —OC3H7)或分枝鏈烷氧基， iv )胺類（一 N R 2 )，及 v )乙酸酯（一〇c〇R，例如一〇C〇C F 3 )。 根據本發明之一具體實例，X -配體係爲前述化合物 之組合物。因此，鉻來源材料視情況係爲
Cp2Zr (〇只，"）乂（：121或〇0221'(：111)。 以下X與R之較佳組合亦可使用於本發明： X = R = C 1或B r，即化合物係爲四鹵化物， X二R = 0 R ” ，即化合物係爲烷醇鉻， x=R=Cp，即化合物係爲四環戊二烯鉻，及/或 X=R=二酮酸酯，由氧配位，具有通式（冚）。 本發明所使用之锆來源材料以四氯化锆（z r c 1 4 ) 或二氯化二環戊二烯基鉻（Cp2ZrCl2)。 經濟部智慧財產局員工消費合作社印製
3 .氧來源材I 氧來源材料可爲任何可使用於A L E技術中之氧化合 物。較佳氧來源材料係包括水、氧及過氧化氫，及過氧化 氫之水溶液。臭氧（〇3 )係爲特佳之氧來源材料，亦爲與 氧（〇2 )之混合物形式。由文獻已知，若使用臭氧作爲氧 之先質’則自形成氧化物得到較致密之材料層，而改善氧 本紙張尺度適用中國國家標準（CNS ) A4規格（21〇χ 297公釐） -17· 567584 A7 ___ B7 五、發明説明（15) 化物薄膜之電容率。 亦可使用以下化合物之一或多種作爲氧之先質： 一氮之氧化物，諸如N2〇、N〇及N〇2， 一鹵化物一氧化合物，例如二氧化氯（C丨〇2 )及過 氯酸（H C 1〇4 )， 一過酸（一〇一〇一Η ),例如過苄酸（ C6H5C〇〇〇H)及過乙酸（CH3C〇〇〇H)， 一醇鹽， 一醇類，5者如甲醇（C Η 3〇Η ),及乙g亨（ c Η 3 c Η 2 〇 Η )，及 一各種基團，例如氧基團（〇.‘）及經基（·〇Η) 〇 根據本發明較佳具體實例，γ s Ζ薄膜係藉A L D式-方法使用Y ( t h d ) 3作爲釔來源材料、二氯化二環戊二 烯基鉻（Cp2Z r C 12)作爲鉻來源材料且臭氧或〇3 與〇2之混合物作爲氧來源材料而生長。 根據另一較佳具體實例，γ S Z薄膜係藉A l D式方 法使用Y ( t h d ) 3作爲釔來源材料、臭氧或〇3與〇2 之混合物作爲氧來源材料、且四氯化鉻（Z r c 1 4 )作爲 錯來源材料且水作爲氧來源材料而生長。 以下貫施例係用以進一步說明本發明。 實施例 貫I双條件及分析設備 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） (請先閱讀背面之注意事項再填寫本頁) 訂 經濟部智慧財產局員工消費合作社印製 -18- 567584 A7 B7 五、發明説明（16) 實施例中，使用Y ( t h d ) 3及二氯化二環戊二烯基 锆（C P2Z r C 1 2) ( Stream Chemicals )作爲金屬來 (請先閲讀背面之注意事項再填寫本頁) 源材料。Y ( t h d ) 3 係根據 Eisentraut 及 Sievers ( Eisentraut, K. J. and Sievers, R.E., J. Am. Chem. Soc. 87 (1965)，5254 )之教不而製備。來源材料係使用熱解重量 分析（TG/DTA，Seiko SSC 5200 )於1毫巴壓力下進行分 析。 該薄膜係於MC — 1 2 0及F — 1 2 0反應器（ASM Microchemistry 〇y，Espoo, Finland )中生長，使用 N 2 ( 5 · 0，Aga)作爲載體氣體。使用臭氧生成器（Flsher 502)自〇2 (5 . 0，Ag a)產生之臭氧作爲氧化劑。 使用（1 0 0 )取向之矽（Okmetic〇y，Finland )及石灰 玻璃作爲基材。個別氧化釔及氧化鉻之生長係以溫度之函-數檢測，而該來源材料之適用性係藉著使用〇 . 5 - 4秒 範圍內之脈衝施加時間進行實驗而確認。 經濟部智慧財產局員工消費合作社印製 所生長之Y2〇3、Z r〇2及Y S Z薄膜的結晶度及 取向係藉X -射線繞射（XRD，Philips MPD 1 8 80，C u K «)分析。該Y及Z r含量及可能雜質係由X -射線螢光 (XPF，Philips PW 1 480 )使用 UniQuant 4.0 軟體且藉掃描 式電子顯微鏡使用能量分散式X —射線分析（S E Μ -E D X )以STRATA軟體測定。Y S Ζ薄膜亦藉X -射線 光子光譜（XPS，AXIS 165，Kratos Analytical )使用單色 A 1 Κ α輻射分析。同時測定來自區域C 1 s 、〇 ls、Zr 3d及Y 3d之寬幅掃描光譜及HiRes (高 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -19- 567584 A7 B7 __ 五、發明説明（17) 、 解析度）光譜。所測量之試樣的面積約爲1毫米2，而測量 係自數個點進行。 (請先閱讀背面之注意事項再填寫本頁) 薄膜厚度或使用Hitachi U-2000 UV-Vis光譜儀及光學 適配方法測量，如 Y1 i 1 a m m i Μ.及 R a n t a a h ο，T ·於 T h i n S ο 1 i d Films 232 ( 1 993)，56所揭示，或藉顯微光波干涉儀（ Υ2〇3 薄膜）（Sloan Dektak SL3030，Veeco Instruments )使用H C 1溶液蝕刻，於適當之步驟使用光阻（ A Z 1 3 5 0 Η，Η 〇 e c h s t )作爲罩幕而測定。 該薄膜亦藉 Nicolet Magna-IR 750 FT-IR 使用 D T G S 偵測器及DRIFTS輔助設備（Spectra Tech Inc )分析。在 約0 · 5 x 0 . 5厘米2 ( 1 0 0 )矽基材上製備之試樣測 定中一 I R -區光譜，使南畢2厘米解析度及6 4條掃 描線之信號平均値。該背景使用該裝置之擴散校準鏡（ 、
Spectra Tech no: 7004-0 1 5 )測量。具有天然氧化物之矽晶 圓的光譜自試樣光譜扣除。來自水及C〇2殘留物於I R光 譜中產生之干擾係以乾燥空氣沖洗而消除。所測量之光譜 的平坦化係視需要進行。 經濟部智慧財產局員工消費合作社印製 實施例1 氧化釔（Υ2〇3)薄膜之製備及分析 Υ2〇3薄膜係藉ALD方法於2 5 0 — 3 5 0 °C溫度 下生長。Y2〇3薄膜之生長速率係爲〇 . 2 3埃/周期。 就自Y ( t hd) 3生長之Υ2〇3薄膜而言，發現 A L D限幅，於溫度範圍2 5 0 - 3 5 0 °C中長晶速率基 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -20- 567584 Α7 Β7 五、發明説明（18) (請先閱讀背面之注意事項再填寫本頁) 本上保持固定。來源材料溫度係爲1 2 〇 t，脈衝施加時 間在Y ( t h d ) 3爲0 · 8秒，而〇3爲3 · 0秒，每個 來源材料脈衝之後的沖洗皆持續1 . 〇秒。亦表示於圖1 ，其中每個周期中，以埃表示之Y 2〇3長晶速率係以長晶 溫度之函數表不。 圖2表示每個周期中，以埃表示之γ2〇3長晶速率， 以來源材料之脈衝時間的函數表示。該圖顯示當 Y ( t h d ) 3之脈衝施加時間約〇 · 5秒（此實驗中，該 〇3脈衝係保持於1 · 5秒）或更長，而〇3之脈衝施加時 間係約1 · 〇秒或更長（此實驗期間，該γ ( t h d ) 3脈 衝係保持於Ο . 8秒）時，長晶速率基本上保持定値之方 法。釔來源材料之溫度係約1 2 0 t，長晶溫度係3 0 0 °C。每次來源材料脈衝之後的沖洗係由〇 . 8至2 . 0秒> ，隨著增加之脈衝時間而增長。 圖3中，Y2〇3薄膜以毫微米表示之厚度係以反應周 期數之函數表示。薄膜係於3 0 0 t下沉積，來源材料 Y (thd) 3之溫度係爲120°C°Y (thd) 3之脈 經濟部智慧財產局員工消費合作社印製 衝時間係爲0 · 8秒，而〇3係爲3 · 0秒。每次來源材料 脈衝之後的沖洗皆持續1 · 0秒。由圖3發現薄膜之厚度 與長晶周期數成線性相依。 於2 5 0 — 3 5 0°C之ALD限幅中生長之Y2〇3薄 膜係爲（1 0 0 )取向。於高溫下生長之薄膜中，亦偵測' 得（1 1 1 )及（4 4〇）取向。於高於4〇〇°C之溫度 下之長晶產生類似於先前技藝所得之結果（Μόΐβ，H.等人 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ297公釐） -21 - 567584 A7 B7 五、發明説明（19) ，Adv· Mat· Opt· E1· 4 ( 1 994)，3 8 9 )。該薄膜之取向或結 晶度未因該來源材料之脈衝施加時間而改變。 實施例2 氧化鉻（Z r〇2)薄膜之製備及分析 氧化錶薄膜係使用C p 2 Z r C 1 2作爲銷來源材料而 製得。該來源材料之溫度係爲1 4 0 °C。該Z r〇2薄膜可 根據ALD原理於275 — 325 t及於400 — 45〇 °C之溫度下生長。第一個範圍內，得到〇 · 4 8埃/周期 之長晶速率，第二範圍內，長晶速率係爲〇 · 5 3埃/周 期。 於圖4中亦可發現以長晶溫度之函數表示之z r〇2薄 膜之長晶速率。此實驗中，該來源材料C p 2 Z r C 1 2之 溫度係爲1 4 0 — 1 5 0 °C。C p 2 Z r C 1 2之脈衝施加 時間個別係爲0 · 8秒及3 · 0秒。而每次來源材料脈衝 之後的沖洗係持續1 . 0秒。 該來源材料之脈衝施加時間於部分實驗中改變。 1 · 0秒之C p 2 Z r C 1 2脈衝使該基材表面飽和。需有 1 · 5秒之〇3脈衝以完成該反應周期。圖5表示每個周期 以脈衝時間之函數表示之Z r〇2長晶速率，以埃表示。該 長晶溫度係爲3 0 0 °C，而來源材料c p 2 Z r C 1 2之溫 度係爲1 4 0 — 1 5 0 °C。沖洗時間係爲1 · 〇秒。該圖 顯示當C p 2 Z r C 1 2之脈衝時間約〇 · 7秒或更長時（ 此等實驗中，〇3之脈衝時間係爲3 . 〇秒）且當〇3之脈 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ 297公釐） .ί.------·!裳— r請先閱讀背面之注意事項再填寫本頁} 訂 經濟部智慈財產局員工消費合作社印製 -22- 567584 A7 B7 五、發明説明（20) 衝施加時間係爲1 . 5秒或更長時（此等實驗中，該 C p 2 Z r C 1 2之脈衝施加時間係爲〇 · 8秒），長晶速 率基本上保持定値的方法。 圖6中，以毫微米表示之Z r〇2薄膜厚度係以反應周 期數之函數表示。該薄膜係於3 0 0 °C下沉積，來源材料 C pzZ r C 1 2之溫度係爲1 4 0 — 1 5 0°C。而脈衝時 間在C p 2 Z r C 1 2爲〇 · 8秒，而〇3爲3 · 0秒。每 個來源材料脈衝之後的沖洗係持續1 . 〇秒。由圖6發現 薄膜厚度與長晶周期數有線性相依性。 使用X R F分析Z I*〇2薄膜中所含之C 1殘留物。於 250-27下生長於矽或玻璃基材上之薄膜中，含 有約0 · 1重量百分比之C 1 。於300 - 325 °C下生 長之薄膜具有約0 · 0 6 - 0 · 0 7重量百分比之氯含量- 。於高於3 2 5 °C下生長之薄膜，未測得氯，即，氯含量 位於偵測極限之下，即約0 · 0 2重量百分比或更低。 使用XRD分析在不同溫度下生長之Z r〇2薄膜。於 低於3 0 0 °C溫度下生長於矽或玻璃基材上之Z I*〇2薄膜 幾乎爲非晶形。2 7 5 °C下生長之薄膜中僅有極弱之尖峰 ，可解釋爲單斜晶Z r〇2之反射。於3 0 0 t下生長之薄 膜中，該尖峰可確認爲單斜晶或立方晶Z r〇2相之反射。_ 當長晶溫度高達到4 5 0 °C時，單斜晶（—1 1 1 )反射 性更強。而於3 0 0 °C及4 5 0 °C下生長於矽基材上之薄 膜的XRD圖型係出示於圖7中。在3 0 0°C下生長之薄 膜的圖型係下方者。於3 0 〇°C及4 5 0°C下生長之薄膜 本紙張尺度適用中國國家標準（CNS ) A4規格（X 297公釐） ----·裝-- (請先閲讀背面之注意事項再填寫本頁) 訂 經濟部智慧財產局員工消費合作社印製 -23- 567584 A7 _B7__ 五、發明説明（21 ) 的厚度個別係爲1 2 0及9 0毫微米。用以確認該相之縮 寫如下：Μ =單斜晶，C =立方晶。該確認係根據 . J CPDS 卡 36 — 420 ( Joint Committee on Power Diffraction Standards (JCPDS), 1 990 )。 實施例3 經釔安定化之氧化銷薄膜的製備及分析 Y S Z薄膜係於3 0 0 °C溫度下使用不同脈衝施加程 序生長。各個脈衝施加程序中，由Y ( t h d ) 3 -脈衝/ 沖洗/ 0 3 -脈衝/沖洗所構成之脈衝施加序列次數係隨著 脈衝/沖洗所構 由C p 2 Z r C 1 2 —脈衝/沖洗/〇 成之脈衝施加序列次數有關。 該薄膜之品質或長晶速率與先沉積於該基材表面上之 金屬來源材料的選擇無關。 該經釔安定化之氧化鉻的長晶速率係視Y / Z Γ脈衝 施加比而定。若Y s z之長晶速率與個別氧化物之總和長 晶試劑比較，貝脈衝施加比1 : 1下，長晶速率較 經濟部智慈財產局員工消費合作社印製 請 先 閱 讀 背 之 注 意 事 項 再 填 馬 本 頁 自個別氧化物之/長晶速率計算之値高約2 5百分比。當釔 脈衝施加序列之次數增加時，即當該薄膜中之纟乙含量增加 時，長晶速率接近計算値。此亦可由圖9得到結論。 在3 0 0 °C下生長之Y S Z薄膜係爲立方晶系，主要 爲（1 0 0 )取向，但如圖1 0所示，亦偵測到（1 1 1 )、（220)及（311)反射。圖1〇揭示厚度爲 9〇毫微米之YS Z薄膜的XRD圖型。該薄膜係於 本紙張尺度適用中國國家標準（CNS ) A4規格（210 Χ 297公釐） -24- 567584 A7 B7 五、發明説明（22) (請先閱讀背面之注意事項再填寫本頁) 3〇0°C下生長於（1 0 〇 )矽基材上。該Y/Z r脈衝 施加比例係爲1 : 1。該相根據J C P D S -卡3〇一 1 4 6 8確認。X R D圖型中之尖峰位置以釔之濃度爲函 數而變化，因爲單元晶胞之尺寸改變。Y。 ： 5 Z r。. 8 5 〇1.93之（2〇〇）反射之】〇？〇3反射値（卡30— 1468)係爲d=2·571埃。圖11顯示YSZ薄 膜之XRD圖型中（200)尖峰隨Y2〇3/Z r〇2比 例改變而變化之方式。圖1 1中之虛線係爲經由文獻所得 之純氧化物d値繪製之參考線。 於3 0 0 °C下長晶之Y S Z薄膜的氯含量使X R F分 析。於低Y濃度下，該薄膜中C 1含量似乎稍低於基本上 由Z r〇2所構成之薄膜。薄膜中γ2〇3爲20 — 50重 量百分比範圍內時，薄膜中釔含量之增加導致摻入薄膜中-之C 1含量增加。此亦可由圖看出。氯（〇 · 23重 量百分比）於該Y S Ζ薄膜中之最高濃度係於該氧化釔濃 度爲5 0重量百分比時測得。 經濟部智慧財產局員工消費合作社印製 該Y S Ζ薄膜於中_ I R —區中測得之I R —光譜僅 於不同波數下顯示來自矽基材之尖峰。來自Y S Ζ薄膜之 實際尖峰可藉著扣除該S i -基材之I R -光譜而測得（ 比較圖1 3 )。該扣除程序中，於1 1 0 0厘米—1來自 . S 1 -〇鍵結之尖峰未完全消失。圖1 4顯示在釔濃度降 低時，如何在所分析之薄膜中偵測朝向較高波數之不同位 移之方法。Y 2〇3吸收之參考値係爲6 1 3厘米_ 1。 使用X -射線光電子光譜（X P S )分析一系列所生 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -25- 567584 A7 B7 五、發明説明（23) 長之Y2〇3、Z r〇2及YSZ薄膜。該試樣中之Υ203 含量係爲0、3、10、30或1〇〇重量百分比。於表 面上測得少量碳及氧（C〇2 )。此係在空氣中操作之s式樣 的典型。自該表面測量之光譜用以計算表面上之原子組成 ，及原子比Y / Z I*，與X —射線螢光（X R F )測量値 所得之結果比較。此種比較係出現於圖1 5中，其中自 X R F結果所計算之Y 2〇3 / Z r〇2比例係位於X —軸 ，而X P S結果所得之Y / Z r比例係位於y -軸。基於 X R S - H i R e s測量値繪線。 (請先閲讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐） -26-

Claims (1)

  1. 六、申請專利範圍 1 · 一種藉A L D式方法於基材上製造氧化物薄膜之 方法’其中將以下物質之交替氣相脈衝 -至少一種金屬來源材料，及 -至少一種氧來源材料，可與沉積於該基材表面上之 金屬來源材料形成氧化物 進料至反應空間內，與該基材接觸， 其h徵爲纟乙來源材料及錯來源材料係交替地作 來源材料，以於基材上形成經釔安定化之氧化锆（ )薄膜。 2 ·如申請專利範圍第1項之方法，其中該γ 爲金屬 Y S Z S Z薄 0 t：爲 請 先 閣 讀 背 面 之 注 意 事 項 再j 裝 膜係於2 5〇一 5 0 0 °C下生長，以2 7 5 — 4 5 佳，尤其是約2 7 5 - 3 2 5 T：。 3 ·如申請專利範圍第1項之方法，其中金屬來源材 料之脈衝施加周期係由以下步驟組成 -借助惰性載體氣體將金屬來源材料之氣相脈衝進料 至該反應空間內； -使用惰性氣體沖洗該反應空間； 將氧來源材料之氣相脈衝進料至該反應空間內； 訂 經濟部智慧財產局員工消費合作社印製 及 -使用惰性氣體沖洗該反應空間 4 ·如申請專利範圍第1 項中任一項之方法，其 來源材 中該第一脈衝施加周期係使用釔來源材料作爲金屬 料而進行。 5 ·如申請專利範圍第1 - 3項中任一項之方 中該第一脈衝施加周期係使用锆來源材料作爲金屬 法，其 來源材 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐） -27- 567584 A8 B8 C8 D8 六、申請專利範圍 料而進行。 6 ·如申請專利範圍第1 一 3項中任一項之方法，其 中Y 2〇3脈衝施加周期相對於Z r〇2脈衝施加周期之脈 衝施加比係由1 : 1 〇至1 〇 : 1 ,以1 : 5至5 : 1爲 佳，由1 : 3至3 : 1更佳，而約1 ·· 1最佳。 7 ·如申請專利範圍第1 一 3項中任一項之方法，其 中該釔來源材料係選自具有通式（I )或（Π )之材料： Y X a ( I ) Y X 3 B ( Π ) 其中 X係選自下列者之群：由氧配位之二酮（即/3 —二酮 酸酯）、環戊二烯基及環戊二烯基衍生物且B係爲中性加 合配體，其鍵結於來自一或多個原子之中心原子。 8 ·如申請專利範圍第7項之方法，其中b係選自烴 類、含氧烴類諸如醚、及含氮烴類諸如聯吡啶、二氮雜菲 、胺或多胺。 9 ·如申請專利範圍第7項之方法，其中該二酮係具 有通式（m ): (III) 其中 R >及R 〃個別選自直鏈或分枝鏈C i 一 C i q烷基， 尤其是直鏈或分枝鏈Ci — C6烷基，最佳係爲—CH3、 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 寫 本 頁 經濟部智慧財產局員工消費合作社印製
    -28- 567584 A8 B8 C8 D8 六、申請專利範圍 -C (CH3) 3、—CF3&_c (CF3) 3。 1 ο .如申請專利範圍第7項之方法，其中該環戊二 嫌基衍生物係具有通式（IV )： C 5 Η 5 - y R '·’ y 其中 IV ) 經濟部智慧財產局員工消費合作社印製 R’"選自直鏈或分枝鏈Ci—CiQ烷基，以Ci—C6 烷基爲佳，尤其是甲基（一ch3)、乙基、丙基、丁基、 戊基、及具有長碳鏈之烷基、烷氧基、芳基、胺基、氰基 及甲矽烷基，且· y係爲整數1 — 5。 1 1 ·如申請專科範圍第1 一 3項中任一項之方法， 其中該锆來源材料係選自具有通式（V )之化合物： R 2 Z r X 2 (V) 其中 R係爲環戊二烯基（C 5 Η 5 )及環戊二烯基之衍生物 且X係選自鹵基、氫、直鏈或分枝鏈Ci 一 ClQ烷基，以 Cl — C6烷基爲佳，尤其是甲基（一 CH3)、乙基、丙 基、丁基、甲氧基（一 OCH3)及其他直鏈（例如 一〇C3H?)或分枝鏈院氧基、胺類（―NR2)，及乙 酸酯（一〇C〇R ,例如一〇C〇C F 3 )。 1 2 .如申請專利範圍第1 二烯基之衍生物係具有通式（IV ) C 5 Η 5 - y R M，y 其中 項之方法，其中該環戊 IV 請 先 閱 讀 背 面 之 注 意 事 項 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -29- 567584 A8 B8 C8 D8 六、申請專利範圍 R…選自直鏈或分枝鏈Ci— CiQ烷基，以Ci—Ce 火兀基爲佳，尤其是甲基（一 ch3)、乙基、丙基、丁基、 戊基、烷氧基、芳基、胺基、氰基及甲矽烷基，且 y係爲整數1 一 5。 1 3 ·如申請專利範圍第1 1項之方法，其中配體R 係橋連，因此具有結構—R — a — R -，其中A係爲甲基 、具有通式（CH2) η之烷基，η = 2 — 6，以2或3爲 佳’或經取代之烴諸如C ( C Η 3 ) 2。 項中任一項之方法， 4 ·如申請專利範圍第1 =中該氧來源材料係選自水、氧、過氧化氫、過氧化氫水 溶液、臭氧、氮之氧化物、鹵化物一氧化合物、過酸（一 〇〜Η)、醇類、醇鹽、各種含氧之基團及其混合物 〇 · 1 5 .如申請專利範圍第χ _ 3項中任一項之方法， 其中使用Y ( t h d ) 3作爲釔來源材料’二氯化二環戊二 稀基銷（c P2Z r c ! 2)作爲錯來源材料，而〇3或〇3 與0 2之混合物作爲氧來源材料。 經濟部智慧財產局員工消費合作社印製
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FI20000898A (fi) 2001-10-15
US7351658B2 (en) 2008-04-01
US20020042165A1 (en) 2002-04-11
US20080014762A1 (en) 2008-01-17
US20100266751A1 (en) 2010-10-21
FI20000898A0 (fi) 2000-04-14
US20050020092A1 (en) 2005-01-27
US6548424B2 (en) 2003-04-15
US7998883B2 (en) 2011-08-16
US7754621B2 (en) 2010-07-13

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