TWI705970B - 含雙(胺基矽基)烷基胺化合物之用於沉積含矽薄膜的組合物、以及使用彼製造含矽薄膜的方法 - Google Patents

含雙(胺基矽基)烷基胺化合物之用於沉積含矽薄膜的組合物、以及使用彼製造含矽薄膜的方法 Download PDF

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TWI705970B
TWI705970B TW107110762A TW107110762A TWI705970B TW I705970 B TWI705970 B TW I705970B TW 107110762 A TW107110762 A TW 107110762A TW 107110762 A TW107110762 A TW 107110762A TW I705970 B TWI705970 B TW I705970B
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chemical formula
silicon
alkyl
alkenyl
film
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TW201900658A (zh
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金成基
李相道
朴重進
張世珍
楊炳日
朴廷主
李三東
李相益
金銘雲
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南韓商Ｄｎｆ有限公司
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Abstract

本發明提供一種含雙(胺基矽基)烷基胺化合物之用於沉積含矽薄膜的組合物，以及使用該組合物製造含矽薄膜的方法。更具體地說，本發明提供一種用於沉積含矽薄膜的組合物，該組合物含有一種能夠有效地作為含矽薄膜之前驅物的雙(胺基矽基)烷基胺化合物；以及一種使用該組合物製造含矽薄膜的方法。

Description

含雙(胺基矽基)烷基胺化合物之用於沉積含矽薄膜的組合物、以及使用彼製造含矽薄膜的方法
本發明係關於一種用於沉積含矽薄膜的組合物及使用該組合物製造含矽薄膜的方法。更具體地說，本發明係關於一種用於沉積含矽薄膜的組合物，該組合物含有特定化合物(即，雙(胺基矽基)烷基胺化合物)作為用於沉積薄膜的前驅物，以及一種使用該組合物製造含矽薄膜的方法。
含矽薄膜在半導體領域中係由各種沉積製程製造，從而被製造成各種形式，例如：矽薄膜、氧化矽薄膜、氮化矽薄膜、碳氮化矽薄膜、及氮氧化矽薄膜，且含矽薄膜的應用領域可為廣泛的。
尤其，由於氧化矽薄膜及氮化矽薄膜具有顯著優異的阻隔性及抗氧化性，因此氧化矽薄膜及氮化矽薄膜於製造設備時係作為絕緣膜、擴散阻絕層、硬式光罩(hard mask)、蝕刻終止層、種晶層、間隔物、凹溝隔離物(trench isolation)、介金屬介電材料、鈍化層(passivation layer)。 近來，多晶矽薄膜已被用於薄膜電晶體(TFT)、太陽能電池等，且其應用領域逐漸地多樣化。
本領域所熟知之製造含矽薄膜的代表技術有：金屬有機化學氣相沉積(MOCVD)法，係使氣態矽前驅物與反應氣體彼此反應以在基板的表面上形成膜，或者直接使氣態矽前驅物與反應氣體於表面彼此反應以形成膜；以及原子層沉積(ALD)法，係物理性或化學性地吸附氣態矽前驅物，然後注入反應氣體以形成膜。諸如採用上述方法的低壓化學氣相沉積(LPCVD)法、電漿增強化學氣相沉積(PECVD)法、能在低溫進行沉積的電漿增強原子層沉積(PEALD)法等各種製造薄膜技術已被用於製造下一代半導體及顯示裝置的製程，以形成超細圖案以及沉積在奈米尺度厚度下具有均勻及優異性質的超薄膜。
用於形成該含矽薄膜的前驅物之代表實例可包括矽烷、矽烷化合物、胺基矽烷、及烷氧矽烷化合物。其具體實例可包括如二氯矽烷(SiH2Cl2)及六氯二矽烷(Cl3SiSiCl3)之氯化矽烷化合物、三矽烷胺(N(SiH3)3)、雙-二乙基胺基矽烷(H2Si(N(CH2CH3)2)2)、二異丙基胺基矽烷(H3SiN(i-C3H7)2)等。這些前驅物已被用於製造半導體及顯示器的量產製程中。
然而，因裝置的超高整合及長寬比(aspect ratio)的增加所導致的裝置精細度，以及裝置材料的多樣化等緣故，仍需要一種可在期望低溫下形成具有均勻及薄厚度及優異性質之超精細薄膜的方法。因此，使用既有矽前驅物的高溫製程(600℃或更高)下，薄膜的階梯覆蓋性(step coverage)、蝕刻性質、物理性質及電性質會有問題，因而須發展新穎的更 優異的矽前驅物及形成薄膜的方法且已加以研究。
本發明之一目的在於提供一種用於沉積含矽薄膜的組合物，該組合物含有一種能作為含矽薄膜之前驅物的雙(胺基矽基)烷基胺化合物。
本發明之另一個目的在於提供一種使用根據本發明之用於沉積含矽薄膜的組合物製造含矽薄膜的方法。
本發明之另一個目的在於提供一種能作為含矽薄膜之前驅物的雙(胺基矽基)烷基胺化合物。
在一個一般性實施方案中，提供一種用於沉積含矽薄膜的組合物，該組合物含有雙(胺基矽基)烷基胺化合物，作為用於沉積薄膜的前驅物時具有優異物理性質，其中該雙(胺基矽基)烷基胺化合物係如以下化學式1所示。
Figure 107110762-A0202-12-0003-2
(在化學式1中，R為(C1-C7)烷基或(C2-C7)烯基；R1至R4各自獨立為氫、(C1-C7)烷基或(C2-C7)烯基，或者R1與R2及R3與R4各自彼此連結而形成一環；以及 R5至R8各自獨立為氫、鹵素、(C1-C7)烷基或(C2-C7)烯基。)
較佳地，在根據本發明例示性實施態樣之化學式1中，R5至R7可各自獨立為氫、鹵素、(C1-C7)烷基或(C2-C7)烯基，以及R8可為氫。
為了使該組合物具有適用於沉積薄膜的優異性質，根據本發明例示性實施態樣之雙(胺基矽基)烷基胺化合物較佳可由以下化學式2或化學式3所示。
Figure 107110762-A0202-12-0004-3
Figure 107110762-A0202-12-0004-4
(在化學式2或化學式3中，R為(C1-C7)烷基或(C2-C7)烯基；R5至R7各自獨立為氫、鹵素、(C1-C7)烷基或(C2-C7)烯基；R11至R14各自獨立為氫、(C1-C5)烷基或(C2-C5)烯基；以及n及m各自獨立為1至7之整數。)
較佳地，在根據本發明例示性實施態樣之化學式2或化學式3中，R5至R7可各自獨立為氫或(C1-C5)烷基；R11至R14可各自獨立為氫、(C1-C5)烷基或(C2-C5)烯基；以及n及m可各自獨立為1至4之整數。
較佳地，根據本發明例示性實施態樣之化學式1所示之雙(胺基矽基)烷基胺化合物可由以下化學式4或化學式5所示。
Figure 107110762-A0202-12-0005-5
Figure 107110762-A0202-12-0005-6
(在化學式4及化學式5中，R為(C1-C7)烷基或(C2-C7)烯基；R11至R14各自獨立為氫、(C1-C7)烷基或(C2-C7)烯基；R5及R6各自獨立為(C1-C7)烷基或(C2-C7)烯基；以及n及m各自獨立為1至7之整數。)
較佳地，在根據本發明例示性實施態樣之化學式4或化學式5中，R可為(C1-C5)烷基；R5及R6可各自獨立為(C1-C5)烷基；以及n及m可各自獨立為1至4之整數。
較佳地，根據本發明例示性實施態樣之化學式1所示之雙(胺基矽基)烷基胺化合物可由以下化學式6或化學式7所示。
Figure 107110762-A0202-12-0005-7
Figure 107110762-A0202-12-0005-8
(在化學式6及化學式7中，R為(C1-C7)烷基或(C2-C7)烯基；R11至R14各自獨立為氫、(C1-C7)烷基或(C2-C7)烯基；以及n及m各自獨立為1至7之整數。)
較佳地，在根據本發明例示性實施態樣之化學式6或化學式7中，R可為(C1-C5)烷基；R11至R14可各自獨立為氫、(C1-C5)烷基或(C2-C5)烯基；以及n及m可各自獨立為1至4之整數。
根據本發明例示性實施態樣之雙(胺基矽基)烷基胺化合物可選自以下化合物，但不限於此。
Figure 107110762-A0202-12-0006-9
Figure 107110762-A0202-12-0007-10
在另一個一般性實施方案中，提供一種使用上述用於沉積含矽薄膜的組合物製造含矽薄膜的方法。
該用於沉積含矽薄膜的組合物可藉由原子層沉積(ALD)法、化學氣相沉積(CVD)法、金屬有機化學氣相沉積(MOCVD)法、低壓化學氣相沉積(LPCVD)法、電漿增強化學氣相沉積(PECVD)法、或電漿增強原子層沉積(PEALD)法而沉積，且含矽薄膜可為氧化矽(SiO2)薄膜、碳氧化矽(SiOC)薄膜、氮化矽(SiN)薄膜、氮氧化矽(SiON)薄膜、碳氮化矽(SiCN)薄膜、或碳化矽(SiC)薄膜。
更具體地，該製造含矽薄膜的方法可包括：a)將安裝於腔室中之基板的溫度維持於30℃至500℃；b)使該基板與上述用於沉積含矽薄膜的組合物接觸，以將用於沉積含 矽薄膜的組合物吸附於該基板中；以及c)將反應氣體注入至其中吸附有該用於沉積含矽薄膜的組合物的該基板中，以形成含矽薄膜，其中該反應氣體係被50W至1000W之電漿功率所產生電漿活化後提供。
在另一個一般性實施方案中，提供一種上述化學式1所示之雙(胺基矽基)烷基胺化合物。
為了更有效地沉積高品質薄膜，化學式1所示之雙(胺基矽基)烷基胺化合物可由化學式2或化學式3所示。
一種含雙(胺基矽基)烷基胺化合物之用於沉積含矽薄膜的組合物，其在室溫下為液態且作為前驅物具有高揮發性及優異熱穩定性，從而可在低電漿功率及薄膜形成溫度條件下提供一種具有高純度及耐久性的高品質含矽薄膜。
進一步地，在使用根據本發明之使用該用於沉積含矽薄膜的組合物製造含矽薄膜的方法中，即使在低的薄膜形成溫度條件下仍可實現優異的熱穩定性及沉積率、以及優異的應力強度，並且在由此製得的含矽薄膜中，雜質(如碳、氧、及氫)的含量可最小化，從而可製造具有高純度、優異物理性質與電性質、對氟化氫的優異抗性、優異水汽穿透率、以及優異階梯覆蓋性的含矽薄膜。
第1圖為示出量測實施例1及實施例2製得的雙(胺基矽基)烷基胺化合物之蒸氣壓所得的結果的視圖。
第2圖為示出對實施例1及實施例2製得的雙(胺基矽基)烷基胺化合物進行熱重分析所得的結果的視圖。
第3圖為示出於實施例3至5中製得的氧化矽薄膜之沉積薄膜上進行紅外光譜分析所得的結果的視圖。
第4圖為示出於實施例6至9中製得的氮化矽薄膜之沉積薄膜上進行紅外光譜分析所得的結果的視圖。
本發明提供一種含雙(胺基矽基)烷基胺化合物之用於沉積含矽薄膜的組合物，該雙(胺基矽基)烷基胺化合物在室溫下為液態且具有高揮發性及優異熱穩定性，因此可作為用於形成含矽薄膜之有用的前驅物，其中該雙(胺基矽基)烷基胺化合物係如以下化學式1所示。
Figure 107110762-A0202-12-0009-11
(在化學式1中，R為(C1-C7)烷基或(C2-C7)烯基；R1至R4各自獨立為氫、(C1-C7)烷基或(C2-C7)烯基，或者R1與R2及R3與R4各自彼此連結而形成一環；以及R5至R8各自獨立為氫、鹵素、(C1-C7)烷基或(C2-C7)烯基。)
根據本發明之用於沉積含矽薄膜的組合物含有化學式1所示之用於沉積薄膜的前驅物，因此可在低溫下進行薄膜的形成，且同時可易於製造具有高耐久性的高品質薄膜。
進一步地，根據本發明之用於沉積含矽薄膜的組合物含有化學式1所示之用於沉積薄膜的前驅物，該薄膜可在高薄膜沉積速率下沉積，且該薄膜具有優異的應力性質及水汽穿透率。
其原因可為：在用於沉積含矽薄膜的組合物所含有的化學式1所示之雙(胺基矽基)烷基胺化合物中，當具有二個胺基矽基基團及一個烷基或烯基基團作為取代基時，該雙(胺基矽基)烷基胺化合物具有高揮發性及熱穩定性。
較佳地，在根據例示性實施態樣之化學式1中，R5至R7可各自獨立為氫、鹵素、(C1-C7)烷基或(C2-C7)烯基，以及R8可為氫。
較佳地，根據本發明例示性實施態樣之化學式1所示之雙(胺基矽基)烷基胺化合物可由以下化學式2或化學式3所示。
Figure 107110762-A0202-12-0010-12
Figure 107110762-A0202-12-0010-13
(在化學式2或化學式3中，R為(C1-C7)烷基或(C2-C7)烯基；R5至R7各自獨立為氫、鹵素、(C1-C7)烷基或(C2-C7)烯基；R11至R14各自獨立為氫、(C1-C5)烷基或(C2-C5)烯基；以及n及m各自獨立為1至7之整數。)
在根據本發明之化學式2或化學式3所示之雙(胺基矽基)烷基胺化合物中，係經二個胺基矽基之官能基及一個烷基或烯基取代，如此該雙(胺基矽基)烷基胺化合物為熱穩定；以及同時該雙(胺基矽基)烷基胺化合物具有矽氮烷(silazane)主幹，其中在二個胺基矽基之官能基中的至少一個上之至少一個氫原子係未經取代，如此該雙(胺基矽基)烷基胺化合物具有高揮發性同時在室溫下為液態。因此，該矽烷胺化合物可顯著有用地用於形成含矽薄膜。
更具體而言，根據本發明之雙(胺基矽基)烷基胺化合物係為具有矽氮烷主幹的化合物，基本上具有二個胺基矽基之官能基(
Figure 107110762-A0202-12-0011-14
及
Figure 107110762-A0202-12-0011-15
，或
Figure 107110762-A0202-12-0011-16
及
Figure 107110762-A0202-12-0011-17
)，且該等胺基矽基之官能基其中一個中的矽基必須具有含至少一個氫原子的官能基(
Figure 107110762-A0202-12-0011-18
或
Figure 107110762-A0202-12-0011-19
)，如此該雙(胺基矽基)烷基胺化合物作為用於沉積薄膜的前驅物時可具有優異的效果。
較佳地，在根據本發明例示性實施態樣之化學式2或化學式3中，R5至R7可各自獨立為氫或(C1-C5)烷基；R11至R14可各自獨立為氫、(C1-C5)烷基或(C2-C5)烯基；以及n及m可各自獨立為1至4之整數。
更佳地，根據本發明之化學式1所示之雙(胺基矽基)烷基胺化合物可由以下化學式4或化學式5所示。
[化學式4]
Figure 107110762-A0202-12-0012-20
Figure 107110762-A0202-12-0012-21
(在化學式4及化學式5中，R為(C1-C7)烷基或(C2-C7)烯基；R11至R14各自獨立為氫、(C1-C7)烷基或(C2-C7)烯基；以及R5及R6各自獨立為(C1-C7)烷基或(C2-C7)烯基；以及n及m各自獨立為1至7之整數。)
較佳地，在根據本發明例示性實施態樣之化學式4及化學式5中，R可為(C1-C5)烷基；R5及R6可各自獨立為(C1-C5)烷基；以及n及m可各自獨立為1至4之整數。更佳地，該雙(胺基矽基)烷基胺化合物可由化學式4所示，且在化學式4中，R可為(C1-C3)烷基；以及R5及R6可各自獨立為(C1-C3)烷基。
較佳地，根據本發明例示性實施態樣之化學式1所示之雙(胺基矽基)烷基胺化合物可由以下化學式6或化學式7所示。
Figure 107110762-A0202-12-0012-22
[化學式7]
Figure 107110762-A0202-12-0013-23
(在化學式6及化學式7中，R為(C1-C7)烷基或(C2-C7)烯基；R11至R14各自獨立為氫、(C1-C7)烷基或(C2-C7)烯基；以及n及m各自獨立為1至7之整數。)
更佳地，在化學式6及化學式7中，R可為(C1-C5)烷基；R11至R14可各自獨立為氫、(C1-C5)烷基或(C2-C5)烯基；n及m可各自獨立為1至4之整數。較佳地，R可為(C1-C5)烷基；R11至R14可各自獨立為(C1-C5)烷基；以及n及m可各自獨立為1至4之整數。更佳地，該雙(胺基矽基)烷基胺化合物可由化學式6所示，其中在化學式6中，R可為(C1-C3)烷基；以及R11至R14可各自獨立為(C1-C3)烷基。
當根據本發明之雙(胺基矽基)烷基胺化合物的矽氮烷主幹上二個胺基矽基之官能基的矽基基團具有二或四個氫原子時，該雙(胺基矽基)烷基胺化合物作為用於沉積薄膜的前驅物係具有更優異的反應性及熱穩定性，因此可製造更高品質的薄膜。
為了使用於沉積薄膜的前驅物具有更優異的性質，根據本發明例示性實施態樣之化學式4所示之雙(胺基矽基)烷基胺化合物可由以下化學式4-1所示。
Figure 107110762-A0202-12-0013-24
(在化學式4-1中，R為(C1-C7)烷基或(C2-C7)烯基；R1及R2各自獨立為氫、(C1-C7)烷基或(C2-C7)烯基，或者R1與R2各自彼此連結而形成一環；以及R5為(C1-C7)烷基或(C2-C7)烯基。)
為了使用於沉積薄膜的前驅物具有更優異的性質，根據本發明例示性實施態樣之化學式6所示之雙(胺基矽基)烷基胺化合物可由以下化學式6-1所示。
Figure 107110762-A0202-12-0014-25
(在化學式6-1中，R為(C1-C7)烷基或(C2-C7)烯基；以及R1及R2各自獨立為(C1-C7)烷基或(C2-C7)烯基，或者彼此連結而形成一環。)
根據本發明例示性實施態樣之化學式1所示之雙(胺基矽基)烷基胺化合物之具體實例不受限制但可包括以下化合物。
Figure 107110762-A0202-12-0014-26
Figure 107110762-A0202-12-0015-27
根據本發明之用於沉積含矽薄膜的組合物必須含有化學式1所示之雙(胺基矽基)烷基胺化合物作為用於沉積薄膜的前驅物，且該雙 (胺基矽基)烷基胺化合物被包含在該用於沉積含矽薄膜的組合物中的含量可在本領域技藝人士考慮薄膜形成條件、厚度、性質等時可認可的含量範圍內。
於本文中，術語「烷基」指線狀、分支狀、及環狀之飽和及不飽和碳氫化合物，其具有1至7個碳原子，較佳具有1至5個碳原子，且更佳具有1至3個碳原子，其實例可包括甲基、乙基、丙基、異丙基、丁基、異丁基、新丁基、戊基等。
於本文中，術語「鹵素」指鹵素元素，其實例包括氟基、氯基、溴基、及碘基。
於本文中，術語「烯基」作為單獨基團或另一基團的一部分，係指一直鏈、支鏈、或環狀碳氫化合物基團，其具有2至7個碳原子及一或多個碳-碳雙鍵。更佳的烯基為具有2至5個碳原子之低碳烯基。最佳的低碳烯基係一具有大約2至3個碳原子之低碳烯基。進一步地，烯基可在任一可連接點處被取代。烯基之實例包括乙烯基、丙烯基、烯丙基、丁烯基、4-甲基丁烯基。該術語「烯基」及「低碳烯基」包括具有順分子配向及反分子配向或者E分子配向及Z分子配向之基團。
於本文中，用語「R1與R2及R3與R4各自彼此連結而形成一環」包括其中R1與R2彼此連結成環但R3與R4不形成環的狀況；其相反狀況，R1與R2不形成環但R3與R4彼此連結成環；以及R1與R2彼此連結成環且R3與R4彼此連結成環的狀況，其中形成的環可為含N的脂環或芳香環，較佳為脂環。
於本文中，術語「脂環」指在有機化合物中非芳香族化合物之具有環狀鍵結結構的化合物。
根據本發明之化學式1所示之雙(胺基矽基)烷基胺化合物可由任一方法製得，只要該方法為本領域技藝人士所認可。
另外，本發明提供一種使用根據本發明之用於沉積含矽薄膜的組合物製造含矽薄膜的方法。
由於在製造含矽薄膜的方法中，係使用根據本發明之用於沉積含矽薄膜的組合物，該組合物含有化學式1所示之雙(胺基矽基)烷基胺化合物作為前驅物，該雙(胺基矽基)烷基胺化合物在室溫下及正常壓力下為液態且具有高揮發性及優異熱穩定性，從而使得處理上變得容易，得以製造各種薄膜，且即使在低溫及低功率下亦可在高沉積速率下製造具有高純度、優異水汽穿透率、以及優異薄膜應力性質的含矽薄膜。
根據本發明之方法所製造的含矽薄膜具有優異耐久性及電性質，以及對氟化氫具有抗性，且其階梯覆蓋性亦為優異的。
在根據本發明之製造含矽薄膜的方法中，該含矽薄膜可由任一方法形成，只要該方法為本領域技藝人士所認可。然而，較佳地，該含矽薄膜可藉由原子層沉積(ALD)法、化學氣相沉積(CVD)法、金屬有機化學氣相沉積(MOCVD)法、低壓化學氣相沉積(LPCVD)法、電漿增強化學氣相沉積(PECVD)法、或電漿增強原子層沉積(PEALD)法形成，但為了讓薄膜能更容易沉積，且使得製造的薄膜具有優異性質，PECVD、ALD、或PEALD是更佳的。
根據本發明之含矽薄膜可為氧化矽(SiO2)薄膜、碳氧化矽(SiOC)薄膜、氮化矽(SiN)薄膜、氮氧化矽(SiON)薄膜、碳氮化矽(SiCN)薄膜、或碳化矽(SiC)薄膜，且可製造具有高品質的各種薄膜， 特別是可用作有機發光二極體(OLED)之封裝材料的薄膜。
更具體地，根據本發明之製造含矽薄膜的方法可包括：a)將安裝於腔室中之基板的溫度維持於30℃至500℃；b)使該基板與根據本發明之用於沉積含矽薄膜的組合物接觸，以將用於沉積含矽薄膜的組合物吸附於該基板中；以及c)將反應氣體注入至其中吸附有該用於沉積含矽薄膜的組合物的該基板中，以形成含矽薄膜。
更具體地，根據本發明之製造含矽薄膜的方法可包括：A)將安裝於腔室中之基板的溫度維持於30℃至500℃；B)使該基板與根據本發明之用於沉積含矽薄膜的組合物接觸，以將該組合物吸附於該基板中；C)沖洗(purging)剩下的用於沉積含矽薄膜的組合物及副產物；D)將反應氣體注入至其中吸附有該用於沉積含矽薄膜的組合物的該基板中，以形成含矽薄膜；以及E)沖洗剩下的反應氣體及副產物，其中步驟D)中的反應氣體可除去用於沉積含矽薄膜的組合物中所含之該雙(胺基矽基)烷基胺化合物的配位基，以形成Si-O原子層。
較佳地，根據本發明例示性實施態樣之反應氣體可被50W至1000W之電漿功率所產生電漿活化後提供。
在根據本發明例示性實施態樣之製造含矽薄膜的方法中，係使用根據本發明之雙(胺基矽基)烷基胺化合物作為前驅物，使得反應氣體較佳在30℃至500℃下，更佳在30℃至300℃下，可被在50W至1000W，較 佳100W至800W，更佳400W至600W的低電漿功率下所產生電漿活化，從而可製造該薄膜。
在根據本發明例示性實施態樣之製造含矽薄膜的方法中，沉積條件可視期望之薄膜的結構或熱性質調整。根據本發明例示性實施態樣之沉積條件的實例可包括：含雙(胺基矽基)烷基胺化合物之用於沉積含矽薄膜的組合物的注入流率、反應氣體及載體氣體的注入流率、壓力、RF功率、該基板的溫度等。作為沉積條件的非限制性實例，用於沉積含矽薄膜的組合物的注入流率可在10立方公分/分鐘至1000立方公分/分鐘的範圍調整；載體氣體的注入流率可在10立方公分/分鐘至1000立方公分/分鐘的範圍調整；反應氣體的注入流率可在1立方公分/分鐘至1500立方公分/分鐘的範圍調整；壓力可在0.5托至10托的範圍調整；RF功率可在50W至1000W的範圍調整；該基板的溫度可在30℃至500℃，較佳80℃至300℃的範圍調整，但沉積條件不限於此。
根據本發明之製造含矽薄膜的方法使用的反應氣體並無限制，但可選自氫氣(H2)、聯氨(N2H4)、臭氧(O3)、氧氣(O2)、一氧化二氮(N2O)、氨(NH3)、氮氣(N2)、矽烷(SiH4)、硼烷(BH3)、二硼烷(B2H6)、及膦(PH3)之一者或前述之二或多者的混合氣體，載體氣體可選自氮氣(N2)、氬(Ar)、及氦(He)之一者或前述之二或多者的混合氣體。
根據本發明之製造含矽薄膜的方法使用的基板可為：含有一或多種選自Si、Ge、SiGe、GaP、GaAs、SiC、SiGeC、InAs、及InP之半導體材料的基板；絕緣體上矽(SOI)基板；石英基板；用於顯示器的玻璃基 板；或可由但不限於聚醯亞胺、聚對苯二甲酸乙二酯(PET)、聚萘二甲酸乙二酯(PEN)、聚甲基丙烯酸甲酯(PMMA)、聚碳酸脂(PC)、聚醚碸(PES)、聚酯等所製之可撓塑膠基板。
進一步地，該含矽薄膜可直接於基板上形成。或者，大部分的導電層、介電層、絕緣層等也可於該基板與該含矽薄膜之間形成。
另外，本發明提供一種能作為含矽薄膜之前驅物的雙(胺基矽基)烷基胺化合物。根據本發明之雙(胺基矽基)烷基胺化合物係由以下化學式1所示。
Figure 107110762-A0202-12-0020-28
(在化學式1中，R為(C1-C7)烷基或(C2-C7)烯基；以及R1至R4各自獨立為氫、(C1-C7)烷基或(C2-C7)烯基，或者R1與R2及R3與R4各自彼此連結而形成一環；以及R5至R8各自獨立為氫、鹵素、(C1-C7)烷基或(C2-C7)烯基。)
根據本發明之雙(胺基矽基)烷基胺化合物由化學式1所示，其如上述在室溫下為液態且具有高揮發性及優異熱穩定性，因此該雙(胺基矽基)烷基胺化合物在形成含矽薄膜中可作為顯著有用的前驅物。
進一步地，由於在各自胺基矽基基團的矽基(矽)中存在四個氫原子，該雙(胺基矽基)烷基胺化合物具有優異反應性，因此可在快速的沉積速率下沉積薄膜，且可製造具有高純度的薄膜。
較佳地，化學式1所示之雙(胺基矽基)烷基胺化合物可由化學式2，且更佳可由化學式6或化學式7所示。
參照以下實施例對本發明進行詳細說明。本說明書及申請專利範圍所用之術語及字詞不應解釋為限於一般意義或字典上的定義，而應基於發明人可適當地定義該術語的概念來最適當地描述他或她所知用於實行本發明之最佳方法的原則下，將之解釋成與本發明技術範圍有關的意義及概念。
因此，在本說明書中之實施態樣中描述及圖式中所示之構型僅為最佳實施例，而非指本發明之所有技術想法，因此應了解的是，可能存在可替代以上構型之多種等效物及改質物。
進一步地，在以下所有實施例中，沉積係使用商業化200毫米單晶圓蓮蓬頭型(shower head type)ALD儀器(CN1,Atomic Premium)藉由本領域所知的電漿增強原子層沉積(PEALD)法進行。另外，沉積係使用商業化200毫米單晶圓蓮蓬頭型CVD(PECVD)儀器(CN1,Atomic Premium)藉由本領域所知的電漿增強化學氣相沉積(PECVD)法進行。
經沉積之含矽薄膜的厚度係使用橢圓偏光計(OPTI-PROBE 2600,THERMA-WAVE)量測，且薄膜的性質係使用紅外光譜(IFS66V/S & Hyperion 3000,Bruker Optics)、X射線光電光譜、水汽穿透率(WVTR)分析儀(MOCON,Aquatran 2)、及應力分析儀(Frontier semiconductor,FSM500TC)分析。
[實施例1]雙(甲基二甲基胺基矽基)甲基胺的製備
Figure 107110762-A0202-12-0022-29
在無水及惰性氣氛下，將二氯甲基矽烷(SiH(CH3)Cl2，115公克(1.0莫耳))及正戊烷(557公克(8莫耳))置入火焰乾燥過的1000毫升燒瓶並慢慢加入甲基胺(CH3NH2，59公克(1.9莫耳))同時維持溫度於-25℃後，攪拌該混合物3小時，然後藉由過濾去除甲基胺基鹽酸鹽((CH3)NH3Cl)。攪拌回收的雙(氯甲基矽基)甲基胺((SiH(CH3)Cl)2N(CH3))溶液及正戊烷並維持溫度於-25℃同時，慢慢加入二甲基胺((CH3)2NH，94公克(7.13莫耳))。添加完成後，該反應溶液慢慢加熱至室溫並於室溫攪拌6小時。在藉由過濾該生成物去除生成的二甲基胺鹽酸鹽((CH3)2NH2Cl，白色)後，獲得一濾液。在減壓下從該濾液中移除溶劑，接著在減壓下蒸餾，從而獲得雙(甲基二甲基胺基矽基)甲基胺(((CH3)2NSiH(CH3))2N(CH3)，71公克(0.35莫耳)，產率：70%)。
1H-NMR(CDCl3)：δ 0.16(t,6H,(Si-CH3)2),2.42(d,3H,(NCH3)),2.48(s,12H,((CH3)2NSi)2),4.39(m,2H,(-SiHN)2).
[實施例2]雙(乙基甲基胺基矽基)甲基胺的製備
Figure 107110762-A0202-12-0022-30
在無水及惰性氣氛下，將二氯矽烷(SiH2Cl2，360公克(3.56莫耳))及正戊烷(3,202公克(27.79莫耳))置入火焰乾燥過的5000毫升不鏽鋼(Sus)反應器(高壓反應器)並慢慢加入甲基胺(CH3NH2，210公克(6.77莫耳))同時維持溫度於-25℃後，攪拌該混合物3小時，然後藉由過 濾去除甲基胺鹽酸鹽((CH3)NH3Cl)。攪拌回收的雙(氯矽基)甲基胺((SiH2Cl)2N(CH3))溶液及正戊烷並維持溫度於-25℃同時，慢慢加入乙基甲基胺((CH3CH2)(CH3)NH，421公克(7.13莫耳))。添加完成後，該反應溶液慢慢加熱至室溫並於室溫攪拌6小時。在藉由過濾該生成物去除生成的乙基甲基胺鹽酸鹽((CH3CH2)(CH3)NH2Cl，白色)後，獲得一濾液。在減壓下從該濾液中移除溶劑，接著在減壓下蒸餾，從而獲得雙(乙基甲基胺基矽基)甲基胺(((CH3CH2)(CH3)NSiH2)2N(CH3)，219公克(1.07莫耳)，產率：60%)。
1H-NMR(C6D6)：δ 0.97(t,6H,(N-CH2-CH3)2),2.47(s,6H,(Si-NCH3)2),2.53(s,3H(SiH2-NCH3)),2.81(q,4H,(N-CH2-CH3)2),4.77(m,4H,(-SiH2N)2).
[實施例3]使用雙(乙基甲基胺基矽基)甲基胺藉由PEALD製造氧化矽薄膜
薄膜係使用根據本發明實施例2製備之雙(乙基甲基胺基矽基)甲基胺作為用於形成氧化矽薄膜的組合物，在一般的電漿增強原子層沉積(PEALD)儀器中使用本領域所知的電漿增強原子層沉積(PEALD)法而形成。
作為反應氣體，一氧化二氮係連同電漿一起使用，以及將對應於惰性氣體之氮氣用於沖洗。於反應氣體及0.5秒的電漿時間形成該薄膜。具體的沉積氧化矽薄膜之方法顯示於表1。
分析所製造氧化矽薄膜所得的結果顯示於表2，以及使用紅外光譜分析沉積的薄膜所得的結果顯示於第3圖。
[實施例4及實施例5]使用雙(乙基甲基胺基矽基)甲基胺 藉由PEALD製造氧化矽薄膜
除了改變如以下表1實施例3所示的沉積條件外，氧化矽薄膜係以與實施例3相同的方法製造，分析所製造氧化矽薄膜所得的結果顯示於以下表2，以及使用紅外光譜分析沉積的薄膜所得的結果顯示於第3圖。
Figure 107110762-A0202-12-0024-31
Figure 107110762-A0202-12-0025-32
[實施例6]使用雙(乙基甲基胺基矽基)甲基胺藉由PEALD製造氮化矽薄膜
薄膜係使用根據本發明實施例2製備之雙(乙基甲基胺基矽基)甲基胺作為用於形成氮化矽薄膜的組合物，在一般的電漿增強原子層沉積(PEALD)儀器中使用本領域所知的電漿增強原子層沉積(PEALD)法而形成。作為反應氣體，氮氣及氨係連同電漿一起使用作為第一反應氣體，以及氮氣係使用作為第二反應氣體。將對應於惰性氣體之氮氣用於沖洗。具體的沉積氮化矽薄膜之方法顯示於表3。
分析氮化矽薄膜所得的具體結果顯示於表4，以及使用紅外光譜分析沉積的薄膜所得的結果顯示於第4圖。
[實施例7至實施例9]使用雙(乙基甲基胺基矽基)甲基胺藉由PEALD製造氮化矽薄膜
除了改變如以下表3實施例6所示的條件外，氮化矽薄膜係以與實施例6相同的方法製造，分析所製造氮化矽薄膜所得的結果顯示於以下表4，以及使用紅外光譜分析沉積的薄膜所得的結果顯示於第4圖。
Figure 107110762-A0202-12-0026-33
Figure 107110762-A0202-12-0026-34
Figure 107110762-A0202-12-0027-35
Figure 107110762-A0202-11-0002-1

Claims (13)

  1. 一種用於沉積含矽薄膜的組合物，該組合物包含雙(胺基矽基)烷基胺化合物，該雙(胺基矽基)烷基胺化合物係由以下化學式2或化學式3所示：
    Figure 107110762-A0305-02-0030-1
    Figure 107110762-A0305-02-0030-2
     在化學式2或化學式3中，R為C1-C3烷基或C2-C3烯基；R5至R7各自獨立為氫、鹵素、C1-C7烷基或C2-C7烯基；R11至R14各自獨立為氫、C1-C3烷基或C2-C3烯基；以及n及m各自獨立為1至7之整數。
  2. 如請求項1所述之組合物，其中在化學式2或化學式3中，R5至R7各自獨立為氫或C1-C7烷基；R11至R14各自獨立為氫、C1-C3烷基或C2-C3烯基；以及n及m各自獨立為1至4之整數。
  3. 如請求項1所述之組合物，其中該雙(胺基矽基)烷基胺化合物係由以下化學式4或化學式5所示：[化學式4]
    Figure 107110762-A0305-02-0031-3
    Figure 107110762-A0305-02-0031-4
     在化學式4及化學式5中，R為C1-C3烷基或C2-C3烯基；R11至R14各自獨立為氫、C1-C3烷基或C2-C3烯基；R5及R6各自獨立為C1-C7烷基或C2-C7烯基；以及n及m各自獨立為1至7之整數。
  4. 如請求項3所述之組合物，其中在化學式4及化學式5中，R為C1-C3烷基；R5及R6各自獨立為C1-C5烷基；以及n及m各自獨立為1至4之整數。
  5. 如請求項1所述之組合物，其中該雙(胺基矽基)烷基胺化合物係由以下化學式6或化學式7所示：
    Figure 107110762-A0305-02-0031-5
    Figure 107110762-A0305-02-0031-6
     在化學式6及化學式7中，R為C1-C3烷基或C2-C3烯基；R11至R14各自獨立為氫、C1-C3烷基或C2-C3烯基；以及n及m各自獨立為1至7之整數。
  6. 如請求項5所述之組合物，其中在化學式6及化學式7中，R為C1-C3烷基；R11至R14各自獨立為氫、C1-C3烷基或C2-C3烯基；以及n及m各自獨立為1至4之整數。
  7. 如請求項1所述之組合物，其中該雙(胺基矽基)烷基胺化合物係選自以下化合物：
    Figure 107110762-A0305-02-0032-9
    Figure 107110762-A0305-02-0033-11
  8. 一種製造含矽薄膜的方法，其係使用如請求項1至7中任一項所述之組合物。
  9. 如請求項8所述之方法，其中，藉由原子層沉積法、化學氣相沉積法、金屬有機化學氣相沉積法、低壓化學氣相沉積法、電漿增強化學氣相沉積法、或電漿增強原子層沉積法進行沉積。
  10. 如請求項8所述之方法，其中該含矽薄膜係氧化矽薄膜、碳氧化矽 (silicon oxy carbide)薄膜、氮化矽薄膜、氮氧化矽薄膜、碳氮化矽薄膜、或碳化矽薄膜。
  11. 如請求項8所述之方法，包含：a)將安裝於腔室中之基板的溫度維持於30℃至500℃；b)使該基板與如請求項1至7中任一項所述之組合物接觸，以將該組合物吸附於該基板中；以及c)將反應氣體注入至其中吸附有該組合物的該基板中，以形成含矽薄膜。
  12. 如請求項11所述之方法，其中該反應氣體係被50W至1000W之電漿功率所產生電漿活化後提供。
  13. 一種由化學式2或化學式3所示之雙(胺基矽基)烷基胺化合物：
    Figure 107110762-A0305-02-0034-7
    Figure 107110762-A0305-02-0034-8
     在化學式2或化學式3中，R為C1-C3烷基或C2-C3烯基；R5至R7各自獨立為氫、鹵素、C1-C7烷基或C2-C7烯基；R11至R14各自獨立為氫、C1-C3烷基或C2-C3烯基；以及n及m各自獨立為1至7之整數。
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CN110431204A (zh) 2019-11-08
US20200111664A1 (en) 2020-04-09
KR20200090654A (ko) 2020-07-29
US11749522B2 (en) 2023-09-05
US20220139704A1 (en) 2022-05-05
JP2020516067A (ja) 2020-05-28
TW201900658A (zh) 2019-01-01
KR102166730B1 (ko) 2020-10-16
KR20180110612A (ko) 2018-10-10

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