TWI754775B - 利用循環沉積在基材上沉積金屬硫屬化物之方法 - Google Patents

利用循環沉積在基材上沉積金屬硫屬化物之方法 Download PDF

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TWI754775B
TWI754775B TW107132993A TW107132993A TWI754775B TW I754775 B TWI754775 B TW I754775B TW 107132993 A TW107132993 A TW 107132993A TW 107132993 A TW107132993 A TW 107132993A TW I754775 B TWI754775 B TW I754775B
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tin
metal
phase reactant
containing gas
substrate
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TW107132993A
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TW201915213A (zh
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米卡 麥提能
米可 雷鐵娜
瑪庫 雷可拉
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荷蘭商Ａｓｍ智慧財產控股公司
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Abstract

本發明揭露一種使用循環沉積沉積金屬硫屬化物在基板上之方法。該方法可包括使該基材接觸至少一含金屬的氣相反應物及使該基材接觸至少一含硫屬元素的氣相反應物。還提供包括使用本發明的方法所沉積金屬硫屬化物的半導體裝置結構。

Description

利用循環沉積在基材上沉積金屬硫屬化物之方法 〔共同研究協議之各方〕
本說明書主張的發明在於或代表及/或有關於赫爾辛基大學和ASM Microchemistry Oy之間的共同研發協議。在所主張之發明完成時或之前，該共同研發協議已生效，而且所主張之發明是在共同研究協議規範內進行的結果。
本發明通常有關利用循環沉積在基層上沉積金屬硫屬化物(Chalcogenide)之方法，而且尤其是，有關循環沉積二硫化錫(Tin disulfide)或二硫化鍺(Germanium disulfide)。本發明亦有關含有利用循環沉積所形成金屬硫屬化物薄膜的半導體裝置結構。
近年來，由於二維(2D)材料具有潛在改善下一代電子裝置效能，以致對這類材料明顯增加興趣。例如，石墨烯(Graphene)是迄今為止研究最多的2D材料，而且具有高遷移率、透射率、機械強度和彈性。然而，純石墨烯中缺乏帶隙已限制其在諸如電晶體的半導體裝置結構中的效能。這種在石墨烯中的限制刺激對作為石墨烯類似物的替代性2D材料的研究。最近，過渡金屬 硫屬化物，而且尤其是過渡金屬二硫屬化物(Dichalcogenide)，在作為石墨烯的替代物方面已引起明顯性的研究關注。過渡金屬二硫屬化物可具有描述夾在兩層硫屬原子(Chalcogen atom)間過渡金屬的MX2化學計量，其層間的金屬硫屬元素和弱面外范德瓦壁(van der Walls)鍵結之間具有強的面內共價鍵結。
然而，生產2D材料的可擴展、低溫方法很少。目前，塊晶的機械剝離是最常用的形成方法，但是雖然此方法產生良好的品質晶體，但此方法無法生產連續薄膜而且需勞力密集，使得此方法不適用於工業生產。化學氣相沉積(Chemical Vapor Deposition，CVD)已用於沉積2D材料，但是目前用於諸如(例如)二硫化錫(SnS2)的金屬硫屬化物的CVD製程在高於600℃的溫度下操作，而且無法產生連續大面積2D材料。因此，想要能夠在降低沉積溫度和原子級薄膜厚度控制下產生具有適宜帶隙的2D材料的方法。
提供的本發明內容是以簡化形式帶入概念方案。此等概念更詳細地說明於以下揭示之實例具體例的詳細說明中。本概要不欲指出所主張標的物之關鍵特徵或基本特徵，亦不欲用來限制所主張標的物之範疇。
在某些實施例中，提供利用循環沉積在基層上沉積金屬硫屬化物之方法。該方法可包括：使該基材接觸至少一含金屬的氣相反應物，該氣相反應物包含由化學式M-O-C表示的一部分化學結構，其中一個金屬原子鍵結一個氧原子(O)、而且該氧(O)原子鍵結一個碳鍵結(C)原子；及使該基材接觸至少一含有硫屬元素的氣相反應物。本發明的實施例亦提供含有本說明書描述方法所沉積的金屬硫屬化物之半導體裝置結構。
為了概括說明本發明及針對先前技術所達成的優點，本發明的某些目的和優點已在本說明書前面描述。當然，應瞭解，不必然可根據本發明 的任何特定實施例實現所有這些目的或優點。因此，例如，熟習該項技藝者將明白，本發明可採取實現或最佳化如本說明書所教示或建議的一優點或一群優點的方式加以具體實施或實現，而無需實現如本說明書所教示或建議的其他目的或優點。
所有這些實施例的全部都在本說明書揭露本發明的範疇內。熟習該項技藝者將可從下列連同參考附圖的特定實施例詳細描述而更明白這些及其他實施例，本發明並沒有受限於所揭露的任何特定實施例。
100:方法
110:製程步驟
120:製程步驟
130:製程步驟
140:判斷步驟
150:步驟
202:資料
204:資料
206:資料
302:資料
304:資料
306:資料
600:半導體裝置結構
602:矽基材
604:二氧化矽層
606:源極區
608:汲極區
610:金屬硫屬化物薄膜/二硫化錫薄層
612:閘極介電層
614:閘電極
700:反應系統
702:反應室
704:前驅物反應物源
704A:導管
706:前驅物反應物源
706A:導管
708:吹掃氣體源
708A:導管
710:系統操作和控制機構
712:退火處理臺
雖然本說明書總結特別指出及明確主張被視為本發明實施例的專利申請項，但是可從本發明實施例的某些實例描述連同參考附圖可更容易確定本發明之實施例的優點，在附圖中：圖1為示意說明根據本發明之實施例之一示例性循環沉積方法的製程流程圖；圖2示意說明根據本發明之實施例所沉積二硫化錫(Tin dichalcogenide)薄膜的低掠角入射X光繞射(Grazing Incidence X-ray Diffraction，GIXRD)資料。
圖3示意說明根據本發明之實施例所沉積二硫化錫薄膜的進一步低掠角入射X光繞射(GIXRD)資料。
圖4為含有根據本發明之實施例所沉積二硫化錫2D材料之結構的高角環暗場掃射電子顯微鏡(High-angle annular dark-field scanning transmission electron microscopy，HAADF-STEM)圖像。
圖5示意說明從根據本發明之實施例所沉積二硫化錫薄膜獲得的拉曼光譜(Raman spectrum)。
圖6示意說明包含根據本發明之實施例所沉積金屬硫屬化物薄膜的示例性 半導體裝置結構；圖7示意說明根據本發明之實施例之可用於沉積金屬硫屬化物薄膜的示例性反應系統。
雖然下面揭露某些實施例和實例，但熟習該項技藝者將瞭解，本發明超出本發明的具體揭露的實施例及/或用途及其明顯修改和等同物。因此，所揭露本發明的範疇並沒有受到下面描述的特定揭露實施例的限制。
本說明書提供的示意說明沒有意味著任何特定材料、結構或裝置的實際視圖，而是僅為針對描述本發明的實施例之理想化表示。
如本說明書的使用，術語「基材」可意指使用可在其上形成一裝置、一電路或一薄膜的任何基層材料或多個材料。
如本說明書的使用，術語「循環沉積」可意指將前驅物(反應物)順序引入反應室以在基材上方沉積一薄膜，而且包括諸如原子層沉積和循環化學氣相沉積的沉積技術。
如本說明書的使用，術語「原子層沉積(Atomic Layer Deposition，ALD)」可意指在處理室中進行沉積循環週期而最好是複數個連續沉積循環週期之氣相沉積製程。通常，在每個循環週期期間，前驅物被化學吸附到一沉積表面(例如一基材表面或一先前沉積的基層表面，諸如來自一先前ALD循環的材料)，形成一單層或亞單層(Sub-monolayer)，不容易與其他前驅物起反應(即是，自限性反應)。此後，如需要，一反應物(例如另一前驅物或反應氣體)隨後可引入處理室，用於將所述化學吸附的前驅物轉換成在沈積表面上的想要材料。通常，此反應物能夠與前驅物進一步反應。此外，在每個循環期間亦可在化學吸附前驅物的轉換後，使用吹掃步驟從處理室除去過量前驅物及/或 從處理室除去過量的反應物及/或反應副產物。此外，如本說明書使用的術語「原子層沉積」還意指包括由相關術語所指出的製程，諸如「化學氣相原子層沉積」、「原子層磊晶(Atomic Layer Epitaxy，ALE)」、分子束磊晶(Molecular Beam Epitaxy，MBE)、氣態源分子束磊晶或有機金屬分子束磊晶和化學束磊晶，而且在連同前驅物組合物、活性氣體和吹掃(例如惰性載體)氣體的交替脈衝進行時。
如本說明書的使用，術語「循環化學氣相沉積」可意指一基材依次暴露於可在基材上反應及/或分解從而產生想要沉積的兩或多個揮發性前驅物的任何製程。
如本說明書的使用，術語「含硫屬元素的氣相反應物」可意指含有硫屬元素的反應物(前驅物)，其中硫屬元素是來自包含硫、硒和碲的化學週期第VI族的元素。
如本說明書的使用，術語「膜」和「薄膜」可意指藉由本說明書揭露的方法沉積的任何連續或非連續結構和材料。例如，「膜」和「薄膜」可包含2D材料、奈米棒、奈米管或奈米顆粒或甚至部分或全部分子層或部分或整個原子層或原子及/或分子簇。「膜」和「薄膜」可包含具有針孔的材料或層，但仍然是至少部分連續。
如本說明書的使用，術語「部分化學結構」可意指化學化合物之一部分的化學結構，即是小於整個化合物的化學結構。
如本說明書的使用，術語「2D材料」或「二維材料」可意指一、兩或三個原子厚度的奈米級結晶質材料。此外，「2D材料」「二維材料」亦可意指由每單層厚度約三個原子厚度的多個單層結晶質材料組成的序化奈米級結晶質結構。
本發明之實施例可包括利用循環沉積在基材上沉積金屬硫屬化 物的方法，特別是藉由原子層沉積方法沉積二硫化錫(SnS2)薄膜或二硫化鍺(GeS2)薄膜的方法。如一非限制性實例所示，二硫化錫是一具有2D晶體結構的新興材料，類似於眾所周知的過渡金屬二硫屬化合物(Transition Metal Dichalcogenide，TMDC)，諸如(例如)，二硫化鉬(Molybdenum disulfide)(MoS2)。相較於最多研究的2D材料、石墨烯、二硫化錫具有相當大的帶隙(塊體~1.8-2.2eV，單層2.8eV)，這使二硫化錫更適合於半導體裝置結構，諸如(例如)，場效電晶體(Field effect transistor，FET)。有關二硫化錫當作FET元件的通道材料之初步研究已顯示等同於二硫化鉬的電性能，諸如(例如)，高達50-200cm2V-1s-1 and on/off ratios of 106的遷移率和108，的導通/關閉比、以及100AW-1的強光響應度。二硫化錫薄膜的其他可能應用領域包括但沒有限於催化作用、能量儲存和太陽光電。
目前用於形成二硫化錫薄膜的方法不適合於形成高品質的保形低溫薄膜。二硫化錫晶體可使用大塊二硫化錫晶體的機械剝離形成，但是這些方法不適合在適宜基材上使二硫化錫形成原子級的厚度精度。此外，二硫化錫的化學氣相沉積已經過證明，但是這種製程在高沉積溫度(大於600℃)下操作，而且不適合製造奈米級保形薄膜。
諸如循環化學氣相沉積和原子層沉積技術的循環沉積方法本質具可塑性，並且提供原子級精確薄膜厚度控制，這對於沉積高品質2D材料是具決定性。此外，諸如原子層沉積的循環沉積方法的特徵在於保形，因此提供均勻塗覆三維結構的能力。在哈姆(Ham)先生等人的ACS Applied Material Interfaces,5,(2013)8880中，二硫化錫的原子層沉積已經由使用Sn(NMe2)4和H2S分別當作錫和硫屬化物前驅物而獲證明。然而，這種形成二硫化錫的先前技術原子層沉積製程可能有問題。例如，二硫化錫可能需要在窄溫度範圍內沉積，而且需要後沉積退火處理使二硫化錫結晶。此外，Sn(NMe2)4前驅物可能略微不 穩定，這可能在諸如(例如)200mm或300mm基材的大面積基材上方導致不良品質薄膜。
因此，想要能夠在低溫、保形和具有原子厚度精度下沉積金屬二硫屬化合物薄膜的方法。此外，理想包含金屬二硫屬化合物薄膜的半導體裝置結構。
一循環沉積製程的非限制性示例實施例可包括ALD，其中ALD是基於典型的自限反應，因此反應物的循序和交替脈衝用於沉積每沉積循環週期約一個原子(或分子)單層材料。通常選擇沉積條件和前驅物提供自飽和反應，使得一反應物的吸收層留下與相同反應物的氣相反應物不起反應的一表面末端。該基材然後接觸一不同反應物，而與先前末端起反應以能繼續沉積。因此，交替脈衝反應物的每個循環週期不會留下超過約一單層的想要材料。然而，如前述，熟習該項技藝者應明白，在一或多個ALD循環週期中，可沉積一個以上的單層材料，例如，如果儘管該製程的交替本質發生某些氣相反應。
在用於沉積金屬硫屬化物薄膜的ALD型製程中，一沉積循環可包括暴露該基材於一第一反應物；從反應空間除去任何未反應的第一反應物和反應副產物；及暴露該基材於一第二反應物，然後接續一第二除去步驟。所述第一反應物可包含一含金屬前驅物，諸如含錫或含鍺前驅物，而且所述第二反應物可包含一含硫屬元素前驅物。
前驅物可由諸如氬氣(Ar)或氮氣(N2)的惰性氣體分離，以防止反應物之間的氣相反應，而且允許自飽和表面反應。然而，在某些實施例中，可移動該基材使其分別接觸一第一氣相反應物和一第二氣相反應物。因為反應是自飽和，使得可不需要嚴格溫度控制基材和精確劑量控制前驅物。然而，基材溫度最好使附帶的氣體物質不會凝結成單層，或不會在基材表面上分解。在基材接觸下一反應性化學物之前，從基材表面除去過量的化學物和反應副產物(若 存在)，諸如藉由吹掃反應空間或藉由移動基材。利用惰性吹掃氣體可有效將不想要的氣體分子從反應空間排出。可使用真空泵來輔助吹掃製程。
能夠用於沉積或生長薄膜的反應器可用於沉積。這種反應器包括ALD反應器、具有適當設備的CVD反應器以及用於提供前驅物的構件。根據某些實施例，可使用一噴灑頭式反應器。
可使用的適宜反應器的實例包括商用的單基材(或單晶圓)沉積設備，諸如可購自位於美國亞利桑那州鳳凰城的ASM America,Inc.公司和位於荷蘭阿爾梅勒市的ASM Europe B.V.公司的Pulsar®反應器(諸如Pulsar® 2000和Pulsar® 3000和Pulsar® XP ALD)和EmerALD® XP和EmerALD®反應器。其他商用反應器包括來自商標名為Eagle® XP和XP8的ASM Japan K.K.公司(位於日本東京)。在某些實施例中，所述反應器為一空間式ALD反應器，其中基材在製程過程會移動或旋轉。
在某些實施例中，可使用一批式反應器。適宜的批式反應器包括但沒有限於商標名稱A400和A412 PLUS的ASM Europe B.V.公司(位於荷蘭阿爾梅勒市)提供的商用Advance® 400系列反應器。在某些實施例中，可使用一直立批式反應器，其中船形器件在製程期間會旋轉，諸如A412。因此，在某些實施例中，晶圓在製程期間轉動。在其他實施例中，批式反應器包括一小批式反應器，其構成容納10個或更少晶圓、8個或更少晶圓、6個或更少晶圓、4個或更少晶圓或2個晶片。在使用一批式反應器的某些實施例中，晶圓與晶圓的均勻性小於3%(1σ)、小於2%、小於1%或甚至小於0.5%
本說明書描述的沉積方法可選擇性在連接一組合設備工具(Cluster tool)的反應器或反應空間中進行。在一組合設備工具中，因為每個反應空間是專屬於一類型製程，使得可保持每個模塊中的反應空間的溫度恆定，而且相較於每次運行前的基材需被加熱到處理溫度的反應器，此相對改善產量。 此外，在組合設備工具中，可減少需將反應空間泵抽到基材間的想要製程壓力位準的時間。
一獨立反應器可具有一裝載鎖。在這情況下，不必然要在每次進行間冷卻反應空間。在某些實施例中，一用於沉積含薄膜的金屬二硫屬化合物薄膜的沉積製程可包括多個沉積循環週期，例如ALD循環週期。
在某些實施例中，循環沉積製程用於形成金屬硫屬化物薄膜在基材上，而且所述循環沉積製程可為一ALD型製程。在某些實施例中，該循環沉積可為一混合ALD/CVD或循環CVD製程。例如，在某些實施例中，相較於一CVD製程，ALD製程的沉積或生長率可能較低。一增加生長率的方法可為在比通常用於ALD製程的較高基材溫度下操作的方法，造成一化學氣相沉積製程，但仍然利用循序引入前驅物，這種製程可稱為循環CVD。
根據本發明的某些實施例，ALD製程用於形成金屬硫屬化物薄膜在基材上，諸如一積體電路工件。在某些實施例中，每個ALD循環週期可包括兩不同沉積步驟或階段。在沉積循環週期的第一階段(金屬相)中，想要沉積的基材表面接觸一第一氣相反應物，該第一氣相反應物包含至少一含錫(Sn)的氣相反應物或至少一含鍺(Ge)的氣相反應物，其係化學吸附在基材表面上，而在基材表面上形成不超過約一單層的反應物。在沉積循環週期的第二階段(硫屬元素相)中，想要沉積的基材表面接觸一第二氣相反應物，該第二氣相反應物包含至少一含硫屬元素的氣相反應物，其與先前化學吸附的物質起反應形成二硫化錫薄膜。
在某些實施例中，在本說明書亦稱為「金屬化合物」之所述至少一含金屬的氣相反應物可包含由下式表示的一部分化學結構：M-O-C 其中一金屬(M)鍵結一個氧(O)原子，而且該氧(O)原子鍵結一個碳(C)原子。在某些實施例中，該等原子之間的鍵可包含一或多個單鍵，然而，在其他實施例中，該等原子之間的鍵可包含一或多個雙鍵。在本發明的某些實施例中，含金屬的氣相反應物包含一含錫(Sn)氣相反應物或一含鍺(Ge)氣相反應物之至少一者。
在某些實施例中，在本說明書亦稱為「錫化合物」之所述含錫(Sn)氣相反應物或錫(Sn)前驅物可包含至少一含錫(Sn)氣相反應物，其具有由下式表示的一部分化學結構；Sn-O-C其中一個錫(Sn)原子鍵結一個氧(O)原子，而且該氧(O)原子鍵結一個碳(C)原子，其中該等揭露原子之間的鍵可包括單鍵或雙鍵。在本發明的某些實施例中，所述至少一含錫(Sn)氣相反應物是由化學式Sn(OR)x表示，其中R是C1-C5烷基，或R是OCCH3基，而且x是從2至6的整數。如一非限制性實例所示，在某些實施例中，所述含錫(Sn)氣相反應物可包含乙酸錫(IV)(Tin(IV)acetate)(Sn(OAc)4)。如一進一步非限制性實例所示，在某些實施例中，所述含錫(Sn)氣相反應物可包含叔丁氧基錫(IV)(Tin(IV)tert-butoxide)(Sn(OtBu)4)。
在某些實施例中，在本說明書亦稱為「錫化合物」之所述錫(Sn)前驅物可包含至少一含錫(Sn)氣相反應物，其具有由下式表示的一部分化學結構；
Figure 107132993-A0305-02-0012-6
 其中一個錫(Sn)原子鍵結或配位兩個氧(O)原子，而且該氧(O)原子透過一個單 鍵和一個雙鍵形成鍵結一個碳原子(C)，而且R可為烴基(Hydrocarbon group)、取代基或非取代基，諸如C1-C3烷基(Alkyl)，例如-CH3。
在某些實施例中，在本說明書亦稱為「錫化合物」之所述錫(Sn)前驅物可包含一單牙配位子(Monodentate ligand)。在某些實施例中，在本說明書中亦稱為「錫化合物」之所述錫(Sn)前驅物可包含一雙牙配位子(Bidentate ligand)。在某些實施例中，在本說明書亦稱為「錫化合物」之所述錫(Sn)前驅物可包含一多芽配位子(Multidentate ligand)。在某些實施例中，所述錫(Sn)前驅物可不包含一單牙配位子。在某些實施例中，所述錫(Sn)前驅物不是由一單牙配位子組成。在某些實施例中，所述錫(Sn)前驅物可不包含一beta-雙酮基配位子(Betadiketonate ligand)，諸如乙醯丙酮酸鹽(Acetylacetonate，acac)或2,2,6,6-四甲基-3,5-庚二酮酸(thd)配位子。在某些實施例中，錫(Sn)前驅物可不包含兩個比上的beta-雙酮基配位子，諸如乙醯丙酮(acac)或2,2,6,6-四甲基-3,5-庚二酮酸(thd)配位子。在某些實施例中，所述錫(Sn)前驅物可不包含一加合物配位子(Adduct ligand)，然而，在其他實施例中，所述錫(Sn)前驅物可包含一或多個加合物配位子。在某些實施例中，所述錫(Sn)前驅物中的Sn具有+IV的氧化態。在某些實施例中，所述錫(Sn)前驅物中的Sn具有+II的氧化態。在某些實施例中，所述錫(Sn)前驅物中的Sn不具有+II的氧化態。
在某些實施例中，在本說明書亦稱為「錫化合物」之所述錫(Sn)前驅物可包含至少一含錫(Sn)氣相反應物，其具有由下式表示的一部分化學結構；
Figure 107132993-A0305-02-0013-7
 其中一個錫(Sn)原子鍵結或配位兩個氧(O)原子，而且該氧(O)原子透過一個單鍵和一個雙鍵形成鍵結一個碳原子(C)，而且R可是一烴基、取代基或非取代 基，諸如C1-C3烷基，例如-CH3，而且其中L是烴基，諸如烷基，其中烴可以或可不包含雜原子(Heteroatom)(即是，除了C或H之外)。
在某些實施例中，在本說明書亦稱為「錫化合物」之所述錫(Sn)前驅物可包含至少一含錫(Sn)氣相反應物，其具有由下式表示的一部分化學結構；L-Sn-O-C
其中一個錫(Sn)原子鍵結或配位一個氧(O)原子，而且該氧(O)原子鍵結一個碳原子(C)，而且其中L是烴基，諸如烷基，其中烴可以或可不包含雜原子(即是，除了C或H之外)。在某些實施例中，在本說明書亦稱為「錫化合物」之所述錫(Sn)前驅物可包含至少一含錫(Sn)氣相反應物，其具有由下式表示的一部分化學結構；X-Sn-L其中X是鹵化物(Halide)，諸如Cl；或除了含烴配位子之外，而且L是烴基，諸如烷基，其中烴可以或可不包含雜原子(即是，除了C或H之外)。
在某些實施例中，在本說明書亦稱為「錫化合物」之所述錫(Sn)前驅物可包含至少一含錫(Sn)氣相反應物，其具有由下式表示的一部分化學結構；Xy-Sn-Lw-y其中X是鹵化物，諸如Cl；或除了含烴配位子之外，y是從0至w或1至w-1，w是從2至4，而且L是烴基，諸如烷基，其中烴可以或可不包含雜原子(即是，除了C或H之外)。
在某些實施例中，在本說明書亦稱為「錫化合物」之所述錫(Sn)前驅物可包含至少一含錫(Sn)氣相反應物，其具有由下式表示的一部分化學結構； Xy-Sn-L4-y其中X是鹵化物，諸如Cl，或除了含烴配位子之外，y是從0至4或1至3，而且L是烴基，諸如烷基，其中烴可以或可不包含雜原子(即是，除了C或H之外)。
在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可包含含Sn或Ge氣相反應物之至少一者，其具有由下式表示的一部分化學結構；-M-O-C-其中一個金屬原子M(Sn或Ge)鍵結一個氧(O)原子，而且該氧(O)原子鍵結一個碳(C)原子。為了簡化緣故，在本說明書中，Ge前驅物或Ge稱為「金屬化合物」或「金屬」，儘管其亦可分別被認為是一半金屬前驅物或半金屬。在本發明的某些實施例中，所述至少一含金屬的氣相反應物是由化學式M(OR)x表示，其中R是C1-C5烷基，而且x是從2至6的整數，而且M是Ge或Sn。如一非限制性實例所示，在某些實施例中，含金屬的氣相反應物可包含乙酸金屬(IV)(Metal(IV)acetate)(M(OAc)4)。如一進一步非限制性實例所示，在某些實施例中，所述含金屬的氣相反應物可包含叔丁氧基金屬(IV)(Metal(IV)tert-butoxide)(M(OtBu)4)。
在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可包含至少一含金屬(Sn或Ge)的氣相反應物，其具有由下式表示的一部分化學結構；
Figure 107132993-A0305-02-0015-3
 其中一個金屬原子M(Sn，Ge)鍵結或配位兩個氧(O)原子，而且該氧(O)原子透過一個單鍵和一個雙鍵形成鍵結一個碳原子(C)，而且R可為烴基、取代基或非取代基，諸如C1-C3烷基，例如-CH3。
在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可包含一單牙配位子。在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可包含一雙牙配位子。在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可包含一多牙配位子。在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可不包含一單牙配位子。在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物不由一單牙配位子組成。在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可不包含一beta-雙酮基配位子，諸如乙醯丙酮(acac)或2,2,6,6-四甲基-3,5-庚二酮酸(thd)配位子。在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可不包含兩個以上的beta-雙酮基配位子，諸如乙醯丙酮(acac)或2,2,6,6-四甲基-3,5-庚二酮酸(thd)配位子。在某些實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可不包含加合物配位子，而在其他實施例中，在本說明書亦稱為金屬化合物之所述金屬前驅物可包含一或多個加合物配位子。在某些實施例中，所述金屬前驅物中的Sn或Ge具有+IV的氧化態。在某些實施例中，所述金屬前驅物中的Sn或Ge具有+II的氧化態。在某些實施例中，所述金屬前驅物中的Sn或Ge不具有+II的氧化態。
在某些實施例中，暴露該基材於至少一含金屬的氣相反應物可包括在該基材上方的金屬前驅物進行脈衝持續介於約0.01秒和約60秒間、介於約0.05秒和約10秒間或介於約0.1秒和約5.0秒間的時段。此外，在該基材上方的金屬前驅物進行脈衝期間，金屬前驅物的流量可小於2000sccm、小於500sccm或甚至小於100sccm。此外，在該基材上方的金屬前驅物進行脈衝期間，金屬前驅物的流量可為從約1至約2000sccm、從約5至約1000sccm或從約10至約500sccm。
從基材表面可除去過量的金屬前驅物，例如錫(Sn)前驅物和反 應副產物(若存在)，例如藉由使用惰性氣體進行泵抽。例如，在本發明的某些實施例中，該等方法可包括一吹掃循環週期，其中吹掃基材表面持續小於約2.0秒的時段。可借助於一泵抽系統產生的真空而除去過量的金屬前驅物和任何反應副產物。
在沉積循環週期的第二階段(硫屬元素相)，該基材接觸包含至少一含硫屬元素的氣相反應物的一第二氣相反應物。在本發明的某些實施例中，所述至少一含硫屬化物的氣相反應物可包含硫化氫(Hydrogen sulfide)(H2S)、硒化氫(Hydrogen selenide)(H2Se)、二甲基硫(Dimethyl sulfide)((CH3)2S)或二甲基碲(Dimethyl telluride)(CH3)2Te。
熟習該項技藝者將瞭解，任何數量的硫屬元素前驅物可用於本說明書揭露的循環沉積方法中。在某些實施例中，一硫屬元素前驅物選自下列清單：H2S、H2Se、H2Te、(CH3)2S、(NH4)2S、二甲基亞碸(Dimethylsulfoxide)((CH3)2SO)、(CH3)2Se、(CH3)2Te、元素或原子S、Se、Te、含有硫屬元素-氫鍵的其他前驅物，諸如具有化學式R-Y-H的H2S2、H2Se2、H2Te2或硫屬化物(Chalcogenol)，其中R可為取代或非取代烴，最好是C1-C8烷基或取代烷基，諸如一甲矽烷基(Alkylsilyl group)，更好是一直鏈或支鏈C1-C5烷基，而且Y可為S、Se或Te。在某些實施例中，硫屬元素前驅物是具有化學式R-S-H的硫醇(Thiol)，其中R可為取代或非取代烴，最好是C1-C8烷基，最好是直鏈或支鏈C1-C5烷基。在某些實施例中，一硫屬元素前驅物具有化學式(R3Si)2Y，其中R3Si是甲矽烷基，而且Y可為Se或Te。在某些實施例中，一硫屬元素前驅物包含S或Se。在某些實施例中，一硫屬元素前驅物包含S。在某些實施例中，一硫屬元素前驅物可包含元素硫屬元素，諸如元素硫。在某些實施例中，一硫屬元素前驅物不包含Te。在某些實施例中，一硫屬元素前驅物確實包含Se。在某些實施例中，一硫屬元素前驅物是選自包含S、Se或Te的前驅物。在某些實 施例中，一硫屬元素前驅物包含H2Sn，其中n是4至10。
適宜的硫屬元素前驅物可包括任何數量的含硫屬元素的化合物，只要化合物包含至少一硫屬元素-氫鍵即可。在某些實施例中，硫屬元素前驅物可包含硫屬電漿(Chalcogen plasma)、硫屬原子或硫屬基團。在需要高能化硫屬元素前驅物的某些實施例中，可在反應室中或反應室的上游產生電漿。在某些實施例中，硫屬元素前驅物不包含一高能化硫屬元素前驅物，諸如電漿(Plasma)、原子或基團。在某些實施例中，硫屬元素前驅物可包含利用含有硫屬元素-氫鍵(諸如H2S)的硫屬元素前驅物形成的一硫屬元素電漿、硫屬原子或硫屬基團。在某些實施例中，一硫屬元素前驅物可包含一硫屬元素電漿、硫屬原子或硫屬基團，諸如包含硫、硒或碲的電漿，最好是包含硫的電漿。在某些實施例中，電漿、原子或基團包含碲。在某些實施例中，電漿、原子或基團包含硒。在某些實施例中，所述硫屬元素前驅物不包含碲前驅物。
在某些實施例中，該基材暴露於含硫屬元素的氣相反應物可包括在基材上的硫屬元素前驅物(例如硫化氫)進行脈衝持續介於0.1秒和2.0秒、從約0.01秒至約10秒、小於約20秒、小於約10秒或小於約5秒的時段。在基材上方的硫屬元素前驅物進行脈衝期間，取代硫屬元素前驅物的流量可小於50sccm、小於25sccm、小於15sccm或甚至小於10sccm。
包含含硫屬元素前驅物的第二氣相反應物可與殘留在該基材上的含金屬分子起反應。在某些實施例中，所述第二相硫屬元素前驅物可包含硫化氫，而且所述反應可在基材表面上沉積金屬硫屬化合物。
可從基材表面除去過量的第二衍生化學物和反應副產物(若存在)，例如使用吹掃氣體脈衝及/或由泵抽系統產生的真空。吹掃氣體最好是任何惰性氣體，諸如但沒有限於氬(Ar)、氮(N2)或氦(He)。如果介入吹掃(即是，吹掃氣體脈衝)或其他反應物去除步驟，則通常認為一階段緊接續另一階段。
基材交替接觸第一氣相反應物(即是，含金屬的前驅物)和第二氣相反應物(即是，含硫屬元素的前驅物)的沉積循環週期可重複兩或多次，然在沉積到想要的金屬硫屬化物厚度停止。應明白，在本發明的某些實施例中，該基材接觸第一相反應物和第二氣相反應物的順序可使得所述基材先接觸第二氣相反應物，然後接觸第一相氣相反應物。此外，在某些實施例中，循環沉積製程可包括該基材接觸第一氣相反應物(即是，含金屬的前驅物)一或多次，然後該基材接觸第二氣相反應物(即是，含硫屬元素的前驅物)一或多次，而且同樣地，可替代性包括該基材接觸第二氣相反應物接觸一或多次，然後所述基材接觸第一氣相反應物一或多次。此外，本發明的某些實施例可包含非電漿反應物，例如第一和第二氣相反應物本質上不含離子化的反應物質。在某些實施例中，所述第一和第二氣相反應物本質上不含離子化的反應物質、受激物質或自由基物質。例如，所述第一氣相反應物和第二氣相反應物兩者可包含非電漿反應物，以防止對下面的基材造成離子化損壞及由此導致的相關缺陷。
利用含金屬的前驅物和含硫屬元素的前驅物形成金屬硫屬化物薄膜之本說明書描述的循環沉積製程可在具有一加熱基材的ALD或CVD沉積系統中進行。例如，在某些實施例中，方法可包括將基材加熱至介於約80℃和約150℃之間的溫度，或甚至將基材加熱至介於約80℃和約120℃之間的溫度。當然，諸如(例如)ALD反應之類的任何特定循環沉積製程的適宜溫度窗格將取決於有關的表面末端和反應物種類。在本說明書，溫度將隨著所使用前驅物而變化，而且通常是在約700℃或低於此溫度以下。在某些實施例中，對於氣相沉積製程而言，沉積溫度通常是在約100℃或高於此溫度，在某些實施例中，該沉積溫度是介於約100℃和約250℃之間，而且在某些實施例中，該沉積溫度在介於約120℃和約200℃之間。在某些實施例中，沉積溫度是低於約500℃、低於約400℃或低於約300℃。在某些情況下，例如，如果製程中使用其他反應物 或還原劑，則沉積溫度可低於約200℃、低於約150℃或低於約100℃。在某些情況下，沉積溫度可高於約20℃、高於約50℃和高於約75℃。在本發明的某些實施例中，沉積溫度(即是，沉積期間的基材溫度)是約150℃。
在某些實施例中，金屬硫屬化物薄膜的生長率是從約0.005Å/週期至約5Å/週期、從約0.01Å/週期至約2.0Å/週期。在某些實施例中，薄膜的生長率大於約0.05Å/週期、大於約0.1Å/週期、大於約0.15Å/週期、大於約0.20Å/週期、大於約0.25Å/週期或大於0.3Å/週期。在某些實施例中，薄膜的生長率小於約2.0Å/週期、小於約1.0Å/週期、小於約0.75Å/週期、小於約0.5Å/週期或小於約0.2Å/週期。在本發明的某些實施例中，金屬硫屬化物的生長率是約0.18Å/週期。
本發明的實施例可包括可為圖1所示方法100更詳細示意說明的一循環沉積。該方法100可從製程步驟110開始，此步驟包括將基材提供到反應室並將該基材加熱到沉積溫度，例如，該基材可包括一塊體矽基材，該反應室可包括一原子層沉積反應室，而且該基材可被加熱到約150℃的沉積溫度。該方法100可繼續製程步驟120，此步驟包括該基材接觸一含金屬的氣相反應物，例如，該基材可接觸乙酸錫(IV)(Sn(OAc)4)持續約1秒的時段。在該基材接觸所述含金屬的前驅物時，可使用一吹掃/泵抽製程從反應室除去過量的含金屬前驅物和任何副產物。該方法100可繼續製程步驟130，此步驟包括該基材接觸含硫屬元素的氣相反應物，例如，該基材可接觸硫化氫(H2S)持續約4秒的時段。在該基材接觸含硫屬元素的前驅物時，可使用吹掃/泵抽製程從反應室除去過量的含硫屬元素前驅物和任何副產物。
基材交替和循序接觸至少一含金屬的氣相反應物和接觸至少一含硫屬元素的氣相反應物接觸的方法可構成一沉積循環週期。在本發明的某些實施例中，沉積金屬硫屬化物(例如一金屬二硫屬化合物)的方法可包括重複沉 積循環兩或多次。例如，該方法100可繼續判斷步驟140，此步驟判斷是否繼續或退出所述方法100。判斷步驟140是基於沉積的金屬硫屬化物薄膜的厚度進行判定，例如，如果金屬硫屬化物薄膜的厚度不足用於想要的裝置結構，則該方法100可返回製程步驟120，而且該基材接觸一含金屬的氣相反應物及該基材接觸一含硫屬元素的氣相反應物的製程可重複兩或多次。一旦金屬硫屬化物薄膜已沉積到想要的厚度，該方法可從步驟150退出，而且該金屬硫屬化物薄膜可經歷其他製程而形成一裝置結構。
在本發明的某些實施例中，剛沉積的金屬硫屬化物薄膜可為至少部分結晶質。例如，圖2示意說明二硫化錫薄膜的三(3)個非限制性實例的低掠角入射X光繞射(GIXRD)資料，其係在約150℃的沉積溫度下利用所揭露的原子層沉積方法進行沉積，其將乙酸錫(IV)(Sn(OAc)4)當作含錫前驅物使用而且將硫化氫(H2S)當作含硫屬元素的前驅物使用。圖2示意說明的GIXRD資料說明使用不同Sn(OAc)4脈衝週期沉積的二硫化錫薄膜，例如，標示202的資料示意說明使用0.2秒的Sn(OAc)4脈衝週期沉積的二硫化錫薄膜，標示204的資料示意說明使用1秒的Sn(OAc)4脈衝週期沉積的二硫化錫薄膜，而且標示206的資料示意說明使用2秒的Sn(OAc)4脈衝週期沉積的二硫化錫薄膜。三(3)個二硫化錫薄膜的GIXRD資料峰值符合(001)晶體取向。因此，在本發明的某些實施例中，沉積二硫化錫薄膜包括使用優勢的(001)晶體取向來沉積二硫化錫。
圖3示意說明二硫化錫薄膜的三(3)個非限制性實例的GIXRD資料，其是在約150℃的沉積溫度下利用揭露的原子層沉積方法進行沉積，其中使用乙酸錫(IV)(Sn(OAc)4)當作含錫前驅物而且硫化氫(Hydrogen sulfide)(H2S)當作含硫屬元素的前驅物。圖3示意說明的GIXRD資料說明使用不同H2S脈衝週期沉積的二硫化錫薄膜，例如，標示302的資料示意說明使用8秒的H2S脈衝週期沉積的二硫化錫薄膜，標示304的資料示意說明使用4秒的H2S脈衝週期沉積 的二硫化錫薄膜，而且標示306的資料示意說明使用2秒的H2S脈衝週期沉積的二硫化錫薄膜。如先前說明，三(3)個二硫化錫薄膜的GIXRD資料峰值符合(001)晶體取向。此外，GIXRD的峰值隨著增加的H2S脈衝週期而增加強度，這說明二硫化錫薄膜的結晶度隨著增加的H2S脈衝時間而增加。因此，在本發明的某些實施例中，二硫化錫薄膜的沉積包括使含硫屬元素的前驅物(例如H2S)進行脈衝持續大於約2秒、大於約4秒或甚至大於約8秒的時段。
雖然剛沉積的金屬硫屬化物薄膜可為至少部分結晶質，但是金屬硫屬化物薄膜的結晶化在沉積製程期間可能緩慢進行，使得較薄的膜比較厚的膜更可少的結晶質。當金屬硫屬化物薄膜包含小於約10奈米厚度的2D材料時，這可能是問題。因此，在本發明的某些實施例中，可使剛沉積的金屬硫屬化物薄膜進行後沉積退火製程，從而改善金屬硫屬化物薄膜的結晶度。例如，在某些實施例中，沉積金屬硫屬化物的方法亦可更包括在介於約150℃和約300℃之間溫度下的該金屬硫屬化物的後沉積退火處理。在某些實施例中，金屬硫屬化物的退火處理可包括將金屬硫屬化物加熱到約小於800℃、約小於600℃、約小於500℃或甚至約小於400℃的溫度。在某些實施例中，金屬硫屬化物薄膜的後沉積退火處理可在包含硫屬元素的大氣中進行，例如，後沉積退火製程可在包含硫屬化物化合物的環境中進行，例如硫化合物，諸如，一硫化氫(H2S)大氣。在某些實施例中，金屬硫屬化物薄膜的後沉積退火處理可進行持續小於1小時、或小於30分鐘、或小於15分鐘、或甚至小於5分鐘的時段。在某些實施例中，金屬硫屬化物薄膜(諸如二硫化錫薄膜)的後沉積退火處理可在不含有硫屬元素(諸如S、Se或Te)的大氣中進行，例如在惰性氣體環境(諸如N2)、鈍氣(諸如Ar或He)或在含氫的環境(諸如H2或H2/N2環境)。
根據本說明書描述的某些實施例所沉積含有金屬硫屬化物薄膜(諸如(例如)，二硫化錫薄膜)的薄膜可為包含2D材料的連續薄膜。在某些實施 例中，包含根據本說明書描述的某些實施例所沉積金屬硫屬化物薄膜的薄膜在低於約100nm、低於約60nm、低於約50nm、低於約40nm、低於約30nm、低於約25nm、低於約20nm或低於約15nm或低於約10nm或低於約5nm或更低的厚度下可為連續。本說明書提到的連續性可為物理連續性或電連續性。在某些實施例中，薄膜可為物理連續性的厚度可不同於薄膜是電連續性的厚度，而且薄膜可為電連續性的厚度可不相同於薄膜是物理連續性的厚度。
圖4示意說明包括根據本發明之實施例所沉積二硫化錫2D材料之結構的橫截面高角環形暗場掃描透射電子顯微鏡(High-angle annular dark-field scanning transmission electron microscopy，HAADF-STEM)圖像。所述HAADF-STEM圖像示意說明一包含矽基材的結構，其中二氧化矽(SiO2)設置在該矽基材上方而且二硫化錫2D材料設置在二氧化矽上方。該結構可更包括一碳(C)層設置在二硫化錫上方，其中該碳(C)層係施加為成像程序之一部分。圖4清楚說明一結晶質二硫化錫(SnS2)2D材料，其具有一2D晶體結構，且約小於8奈米的厚度。
使用本發明的實施例所沉積的二硫化錫薄膜可包含二硫化錫而且可採用SnSx的形式，其中x的範圍可從約0.75至約2.8，或其中x的範圍可從約0.8至約2.5，或其中x的範圍可從0.9至約2.3，或者其中x的範圍可從約0.95至約2.2。SnSx的元素成份範圍可包含從約30原子%至約60原子%、從約35原子%至約55原子%或甚至從約40原子%至約50原子%的Sn。或者，SnSx的元素成份範圍可包含從約25原子%至約75原子%的S、從約30%至約60原子%的S或甚至從約35原子%至約55原子%的S。
在本發明的某些實施例中，金屬硫屬化物的階段(例如二硫化錫)可利用拉曼光譜法(Raman spectroscopy)測定。例如，圖5示意說明在250℃溫度下的退火處理之後，使用325奈米雷射測量的7奈米厚度二硫化錫薄膜的拉曼 光譜。圖5示意說明的拉曼光譜清楚顯示在313cm-1處(對應於SnS2峰值)的強度峰值。在測量中沒有偵測到來自其他SnSx相(諸如SnS或Sn2S3)的峰值。因此，在本發明的某些實施例中，沉積二硫化錫包括使用SnS2給定的化學計量來沉積二硫化錫薄膜。
在其他實施例中，SnSx可包含小於約20原子%氧、小於約10原子%氧、小於約5原子%氧或甚至小於約2原子%氧。在進一步實施例中，SnSx可包含小於約10原子%氫、小於約5原子%氫、小於約2原子%氫或甚至小於約1原子%氫。在仍然進一步實施例中，SnSx可包含小於約10原子%碳、小於約5原子%碳、小於約2原子%碳、小於約1原子%碳、甚至小於約1原子%碳或甚至小於約0.5原子%碳。在本說明書描述的實施例中，可利用盧瑟福背散射(Rutherford Backscattering，RBS)確定元素的原子濃度。
在本發明的某些實施例中，金屬硫屬化物薄膜可沉積在三維結構上在某些實施例中，在具有大於約2、大於約5、大於約10、大於約25、大於約50或甚至大於約100的縱橫比(高度/寬度)的結構中，金屬硫屬化物薄膜的階梯覆蓋率可等於或大於約50%、大於約80%、大於約90%、約95%、約98%或約99%或更大。
在某些實施例中，根據本說明書描述的某些實施例所沉積的金屬硫屬化物薄膜(諸如包含錫和硫屬元素的二硫化錫薄膜)可為結晶質或多晶體。在某些實施例中，根據本說明書描述的某些實施例所沉積的金屬硫屬化物薄膜可具有從約20nm至約100nm的厚度。在某些實施例中，根據本說明書描述的某些實施例所沉積的金屬硫屬化物薄膜可具有從約20nm至約60nm的厚度。在某些實施例中，根據本說明書描述的某些實施例所沉積的金屬硫屬化物薄膜可具有大於約20nm、大於約30nm、大於約40nm、大於約50nm、大於約60nm、大於約100nm、大於約250nm、大於約500nm或更大的厚度。在某些實 施例中，根據本說明書描述的某些實施例所沉積的金屬硫屬化物薄膜可具有小於約50nm、小於約30nm、小於約20nm、小於約15nm、小於約10nm、小於約5nm、小於約3nm、小於約2nm或甚至小於約1nm的厚度。
在某些實施例中，根據本說明書描述某些實施例所沉積的二硫化錫或二硫化鍺薄膜的金屬硫屬化物薄膜的厚度可具有等於或小於約10個單層金屬硫屬化物材料、等於或小於約7個單層金屬硫屬化物材料、等於或小於約5個單層金屬硫屬化物材料、等於或小於約4個單層金屬硫屬化物材料、等於或小於約3個單層金屬硫屬化物材料、等於或小於約2個單層金屬硫屬化物材料或甚至等於或小於約1單層金屬硫屬化物材料。
使用本說明書揭露的循環沉積製程所沉積的金屬硫屬化物薄膜可用於各種環境中，諸如用於形成半導體裝置結構。熟習該項技藝者將明白，本說明書描述的製程適用於許多環境，包括電晶體製造。
如一非限制性示例所示，而且參考圖6，一半導體裝置結構600可包括一場效電晶體(Field Effect Transistor，FET)，其可包括一矽基材602和一設置在所述矽基材602上方的二氧化矽(SiO2)層604。該半導體裝置結構600亦可包括一源極區606和一汲極區608。設置在源極區和汲極區之間是根據本發明的實施例所沉積金屬硫屬化物薄膜610。金屬硫屬化物的薄膜可包含二硫化錫薄層，而且可由所述FET結構的通道區域組成。在本發明的某些實施例中，所述二硫化錫薄層可具有小於10nm、小於5nm或甚至小於1nm的厚度。該半導體裝置結構600可更包括一設置在二硫化錫薄膜上方的閘極介電層612，其中該閘極介電層612可包含二氧化鉿(Hafnium dioxide)(HfO2)。該半導體裝置結構600可更包括一設置在所述二硫化錫薄層610上方的閘電極614。
本發明的實施例可亦包括一構成用於形成本發明的金屬硫屬化物薄膜之反應系統。更具體地，圖7示意說明一反應系統700包括一反應室 702，該反應室更包括用於在預定壓力、溫度和環境條件下保持一基材(未示出)及用於選擇性暴露該基材於各種氣體的機構。一前驅物反應物源704可藉由導管或其他適宜構件704A耦接到反應室702，而且可進一步耦接到一歧管、閥體控制系統、質量流量控制系統或控制來自前驅物反應物源704的氣態前驅物之機構。由前驅物反應物源704(反應物(未示出))提供的前驅物(未示出)在室溫和標準大氣壓條件下可為液態或固態。這種前驅物可在反應物源真空容器內蒸發，其可保持在一前驅物源腔室內的蒸發溫度或高於蒸發溫度。在這實施例中，蒸發的前驅物可使用一載氣(例如，一非活性氣體或惰性氣體)輸送，然後透過導管704A供給反應室702。在其他實施例中，前驅物在標準條件下可為蒸氣。在這實施例中，前驅物不需要被蒸發而且可不需要一載氣。例如，在一實施例中，前驅物可儲存在氣瓶中。反應系統700可亦包括可藉由如前述導管706A而亦耦接到反應室的其他前驅物反應物源，諸如前驅物反應物源706。
一吹掃氣體源708亦可經由導管708A而耦接到反應室702，而且將各種惰性氣體或鈍氣選擇性供應給反應室702，促成從該反應室去除前驅物氣體或廢氣。可供應的各種惰性氣體或鈍氣可源自於一固態、液態或埋存氣態形式。
圖7所示的反應系統700亦可選擇性包括退火處理臺712，其中金屬硫屬化物經歷後生長退火處理。在某些實施例中，反應室702可執行後生長退火處理，然而，在某些實施例中，可將金屬硫屬化物薄膜轉移(例如在受控大氣下)到退火處理臺712，其中後生長退火處理可在想要的氣體環境下進行。
圖7所示的反應系統700亦可包括提供電子電路和機械組件從而選擇性操作反應系統700所內含閥體、歧管、泵及其他設備之一系統操作和控制機構710。這種電路和組件操作上從對應的前驅物源704、706和吹掃氣體源708引入前驅物、吹掃氣體。所述系統操作和控制機構710亦控制氣體脈衝序列 的時序、基材和反應室的溫度、與反應室的壓力及提供反應系統700的正常操作所需的各種其他操作。所述操作和控制機構710可包括控制軟體和電動或氣動控制閥體，從而控制前驅物、反應物和吹掃氣體流入及流出反應室702的流量。所述控制系統可包括執行某些工作的諸如軟體或硬體組件的模組，例如一FPGA或ASIC。一模組可有利地構成常駐在所述控制系統的可定址儲存媒體上，而且構成執行一或多個製程。
熟習該項技藝者應明白可有本反應系統的其他構造，包括不同數量和類類的前驅物反應物源和吹掃氣體源。此外，熟習該項技藝者將亦明白，具有許多可用於實現將氣體選擇性供應給反應室702的目標之閥體、導管、前驅物源、吹掃氣體源的配置。此外，如一反應系統的示意圖所示，其為了簡化說明，已省略許多組件，而且這些組件可包括(例如)各種閥體、歧管、淨化器、加熱器、容器、通氣口及/或分流。
前述本發明的示例實施例沒有限制本發明的範疇，因為這些實施例僅是本發明的實施例的實例，其是由文後申請專利範圍及其合法的等同專利項所定義。任何等同實施例都在本發明的範圍內。實際上，除了本說明書所示和所述之類以外，熟習該項技藝者可從描述更明白本發明的各種修改，諸如所述元件的替代可用組合。這些修改和實施例亦在文後申請專利範圍的範疇內。
Figure 107132993-A0202-11-0002-13
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130‧‧‧製程步驟
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Claims (24)

  1. 一種使用循環沉積在基板上沉積金屬硫屬化物的方法，該方法包括：使該基材接觸至少一含金屬的氣相反應物，該氣相反應物包含由化學式M-O-C表示的一部分化學結構，其中“M”代表金屬原子，“O”代表氧原子，且“C”代表碳原子；且其中該金屬原子鍵結該氧原子，且該氧原子鍵結該碳原子；及使該基材接觸至少一含硫屬元素的氣相反應物。
  2. 如請求項1所述之方法，其中該金屬硫屬化物包含一金屬二硫屬化合物。
  3. 如請求項1所述之方法，其中該至少一含硫屬元素的氣相反應物包含硫(S)、硒(Se)或碲(Te)。
  4. 如請求項1所述之方法，其中該金屬硫屬化物包含小於10原子%的氧(O)含量。
  5. 如請求項1所述之方法，其中該循環沉積包括原子層沉積。
  6. 如請求項1所述之方法，其中該循環沉積包括循環化學氣相沉積。
  7. 如請求項1所述之方法，其中該含金屬的氣相反應物包括含錫(Sn)的氣相反應物或含鍺(Ge)的氣相反應物之至少一者。
  8. 如請求項7所述之方法，其中該至少一含錫(Sn)的氣相反應物是由化學式Sn(OR)x表示，其中R是C1-C5烷基，而且x是從2至6的整數。
  9. 如請求項7所述之方法，其中該至少一含錫(Sn)的氣相反應物包含乙酸錫(IV)。
  10. 如請求項7所述之方法，其中該至少一含錫(Sn)的氣相反應物是 由以下部分化學式表示：
    Figure 107132993-A0305-02-0031-4
     其中一個錫(Sn)原子鍵結兩個氧(O)原子，而且該氧(O)原子透過一個單鍵和一個雙鍵而鍵結一個碳原子(C)，而且R包含一烴基。
  11. 如請求項7所述之方法，其中該至少一含錫(Sn)的氣相反應物是由以下部分化學式表示：
    Figure 107132993-A0305-02-0031-5
     其中一個錫(Sn)原子鍵結兩個氧(O)原子，而且該氧(O)原子透過一個單鍵和一個雙鍵而鍵結一個碳原子(C)，而且R是一烴基，而L是另一烴基。
  12. 如請求項7所述之方法，其中該至少一含錫(Sn)的氣相反應物是由以下部分化學式表示：L-Sn-O-C其中一個錫(Sn)原子鍵結一個氧(O)原子，而且該氧(O)原子鍵結一個碳原子(C)，而且L是一烴基。
  13. 如請求項1所述之方法，其中該至少一含硫屬元素的氣相反應物包含硫化氫(H2S)、硒化氫(H2Se)、二甲基硫((CH3)2S)或二甲基碲((CH3)2Te)。
  14. 如請求項1所述之方法，其中該方法包括至少一沉積循環週期，其中該基材為交替及循序接觸該至少含金屬的氣相反應物和該至少一含硫屬元素的氣相反應物。
  15. 如請求項14所述之方法，其中該沉積循環週期重複兩或多次。
  16. 如請求項1所述之方法，其更包括將該基材加熱到大於約150℃的溫度。
  17. 如請求項16所述之方法，其更包括將該基材加熱到小於約500℃的溫度。
  18. 如請求項1所述之方法，其中該金屬硫屬化物包含二硫化錫。
  19. 如請求項1所述之方法，其中該金屬硫屬化物包含二硫化鍺。
  20. 如請求項1所述之方法，其更包括在介於約150℃和約300℃之間的溫度下的該金屬硫屬化物的後沉積退火處理。
  21. 如請求項20所述之方法，其中該後沉積退火金屬硫屬化物是在硫化氫(H2S)大氣中進行。
  22. 一種半導體裝置結構，其包含使用如請求項1所述之方法所沉積的金屬硫屬化物。
  23. 如請求項22所述之半導體裝置結構，其中該金屬硫屬化物包括一電晶體結構中的至少一部分通道區。
  24. 一種反應系統，其構成執行如請求項1所述之方法。
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TW201915213A (zh) 2019-04-16
KR20190040480A (ko) 2019-04-18
CN115725952A (zh) 2023-03-03
US10734223B2 (en) 2020-08-04
CN109652785B (zh) 2022-12-06
KR102645979B1 (ko) 2024-03-12

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