CN110431204A - 用于沉积含硅薄膜的含双(氨基甲硅烷基)烷基胺化合物的组合物及使用其制造含硅薄膜的方法 - Google Patents

用于沉积含硅薄膜的含双(氨基甲硅烷基)烷基胺化合物的组合物及使用其制造含硅薄膜的方法 Download PDF

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CN110431204A
CN110431204A CN201880019422.XA CN201880019422A CN110431204A CN 110431204 A CN110431204 A CN 110431204A CN 201880019422 A CN201880019422 A CN 201880019422A CN 110431204 A CN110431204 A CN 110431204A
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alkyl
chemical formula
alkenyl
silicon
film
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CN110431204B (zh
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金成基
朴廷主
朴重进
张世珍
杨炳日
李相道
李三东
李相益
金铭云
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DNF Co Ltd
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DNF Co Ltd
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    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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Abstract

提供了用于沉积含硅薄膜的含有双(氨基甲硅烷基)烷基胺化合物的组合物以及使用其制造含硅薄膜的方法，且更具体地，提供了用于沉积含硅薄膜的含有能够有用地用作含硅薄膜的前体的双(氨基甲硅烷基)烷基胺化合物的组合物，以及使用该组合物制造含硅薄膜的方法。

Description

用于沉积含硅薄膜的含双(氨基甲硅烷基)烷基胺化合物的组 合物及使用其制造含硅薄膜的方法
技术领域
本发明涉及用于沉积含硅薄膜的组合物和使用该组合物制造含硅薄膜的方法，并且更具体地，涉及用于沉积含硅薄膜的含有特定化合物——双(氨基甲硅烷基)烷基胺化合物作为用于沉积薄膜的前体的组合物，以及使用该组合物制造含硅薄膜的方法。
背景技术
含硅薄膜是通过半导体领域中的各种沉积工艺制造的，从而被制造成各种形式，诸如硅膜、氧化硅膜、氮化硅膜、碳氮化硅膜和氧氮化硅膜，并且含硅薄膜的应用领域可以很宽。
特别地，由于氧化硅膜和氮化硅膜具有显著优异的阻挡性和抗氧化性，所以氧化硅膜和氮化硅膜在制造装置中被用作绝缘膜、扩散阻挡层、硬掩模、蚀刻停止层、种子层、间隔物、沟槽隔离、金属间介电材料和钝化层。
近来，多晶硅薄膜已经用于薄膜晶体管(TFT)、太阳能电池等，且其应用领域已逐渐多样化。
作为本领域已知的用于制造含硅薄膜的代表性技术，存在使气体型硅前体和反应气体彼此反应以在基底的表面形成膜或使气体型硅前体和反应气体直接在表面上彼此反应以形成膜的金属有机化学气相沉积(MOCVD)方法，以及物理或化学吸附气体型硅前体并且相继注入反应气体以形成膜的原子层沉积(ALD)方法。用于制造薄膜的各种技术，诸如应用上述方法的低压化学气相沉积(LPCVD)法、能够在低温下进行沉积的等离子体增强化学气相沉积(PECVD)法和等离子体增强原子层沉积(PEALD)方法等，被应用于制造下一代半导体和显示器件的工艺，从而用于形成超精细图案并以纳米级厚度沉积具有均匀和优异性能的超薄膜。
用于形成含硅薄膜的前体的代表性实例可包括硅烷、硅烷化合物、氨基硅烷和烷氧基硅烷化合物。其具体实例可包括氯硅烷化合物，诸如二氯硅烷(SiH2Cl2)和六氯乙硅烷(Cl3SiSiCl3)、三甲硅烷基胺(N(SiH3)3)、双二乙基氨基硅烷(H2Si(N(CH2CH3)2)2)、二异丙基氨基硅烷(H3SiN(i-C3H7)2)等。这些前体已用于制造半导体和显示器的批量生产工艺中。
然而，由于器件的超高集成度引起的器件精细度和宽高比的增加以及器件材料的多样化，需要形成具有所期望的均匀和薄的厚度和低温下优异的电性质的超精细薄膜的技术。因此，使用现有硅前体的高温工艺(600℃或更高)，薄膜的台阶覆盖、蚀刻性能以及物理和电性质已成为问题，从而研究了开发新型更优异的硅前体以及形成薄膜的方法。
发明内容
技术问题
本发明的目的是提供用于沉积含硅薄膜的组合物，该组合物含有能够用作含硅薄膜的前体的双(氨基甲硅烷基)烷基胺化合物。
本发明的另一目的是提供使用根据本发明的用于沉积含硅薄膜的组合物制造含硅薄膜的方法。
本发明的另一目的是提供能够用作含硅薄膜的前体的双(氨基甲硅烷基)烷基胺化合物。
问题解决方案
在一个总的方面，提供了用于沉积含硅薄膜的组合物，该组合物含有：作为含硅薄膜沉积的前体的双(氨基甲硅烷基)烷基胺化合物，其作为薄膜沉积的前体具有优异的物理性质，其中双(氨基甲硅烷基)烷基胺化合物由以下化学式1表示。
[化学式1]
(在化学式1中，
R是(C1-C7)烷基或(C2-C7)烯基；
R1至R4各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基，或R1和R2以及R3和R4各自独立地相互连接形成环；以及
R5至R8各自独立地为氢、卤素、(C1-C7)烷基或(C2-C7)烯基。)
优选地，在根据本发明示例性实施方式的化学式1中，R5至R7可各自独立地为氢、卤素、(C1-C7)烷基或(C2-C7)烯基，以及R8可为氢。
为了使组合物具有适合于薄膜沉积的优异性能，优选根据本发明示例性实施方式的双(氨基甲硅烷基)烷基胺化合物可以由以下化学式2或3表示。
[化学式2]
[化学式3]
(在化学式2或3中，
R是(C1-C7)烷基或(C2-C7)烯基；
R5至R7各自独立地为氢、卤素、(C1-C7)烷基或(C2-C7)烯基；
R11至R14各自独立地为氢、(C1-C5)烷基或(C2-C5)烯基；以及
n和m各自独立地为1至7的整数。)
优选地，在根据本发明示例性实施方式的化学式2或3中，R5至R7可各自独立地为氢或(C1-C5)烷基；R11至R14可各自独立地为氢、(C1-C5)烷基或(C2-C5)烯基；以及，n和m可各自独立地为1至4的整数。
优选地，根据本发明示例性实施方式的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物可以由以下化学式4或5表示。
[化学式4]
[化学式5]
(在化学式4和5中，
R是(C1-C7)烷基或(C2-C7)烯基；
R11至R14各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基；
R5和R6各自独立地为(C1-C7)烷基或(C2-C7)烯基；以及
n和m各自独立地为1至7的整数。)
优选地，在根据本发明示例性实施方式的化学式4或5中，R可以是(C1-C5)烷基；R5和R6可各自独立地为(C1-C5)烷基；以及，n和m可各自独立地为1至4的整数。
优选地，根据本发明示例性实施方式的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物可以由以下化学式6或7表示。
[化学式6]
[化学式7]
(在化学式6和7中，
R是(C1-C7)烷基或(C2-C7)烯基；
R11至R14各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基；以及
n和m各自独立地为1至7的整数。)
优选地，在根据本发明示例性实施方式的化学式6或7中，R可以是(C1-C5)烷基；R11至R14可各自独立地为氢、(C1-C5)烷基或(C2-C5)烯基；以及，n和m可各自独立地为1至4的整数。
根据本发明示例性实施方式的双(氨基甲硅烷基)烷基胺化合物可选自以下化合物，但不限于此。
在另一总体方面，提供了使用上述用于沉积含硅薄膜的组合物制造含硅薄膜的方法。
用于沉积含硅薄膜的组合物可以通过原子层沉积(ALD)方法、化学气相沉积(CVD)方法、金属有机化学气相沉积(MOCVD)方法、低压化学气相沉积(LPCVD)方法、等离子体增强化学气相沉积(PECVD)方法或等离子体增强原子层沉积(PEALD)方法来沉积，并且含硅薄膜可以是氧化硅(SiO2)膜、碳氧化硅(SiOC)膜、氮化硅(SiN)膜、氮氧化硅(SiON)膜、碳氮化硅(SiCN)膜或碳化硅(SiC)膜。
更具体地，用于制造含硅薄膜的方法可包括：a)将安装在腔室中的基底的温度保持在30至500℃；
b)使上述用于沉积含硅薄膜的组合物与基底接触，以将用于沉积含硅薄膜的组合物吸附在基底中；以及
c)将反应气体注入至其中吸附了用于沉积含硅薄膜的组合物的基底以形成含硅薄膜，其中，在通过产生等离子体功率为50至1000W的等离子体而激活反应气体之后，供应反应气体。
在另一总体方面，提供了由上述化学式1表示的双(氨基甲硅烷基)烷基胺化合物。
为了更有效地沉积高质量薄膜，由化学式1表示的双(氨基甲硅烷基)烷基胺化合物可以由化学式2或3表示。
发明的有益效果
用于沉积含硅薄膜的组合物含有作为前体的双(氨基甲硅烷基)烷基胺化合物，该化合物在室温下是液体并且具有高挥发性和优异的热稳定性，使得可以在较低的等离子体功率和成膜温度条件下提供具有高纯度和耐久性的高质量含硅薄膜。
此外，在使用根据本发明的用于沉积含硅薄膜的组合物制造含硅薄膜的方法中，即使在低成膜温度条件下也可以实现优异的热稳定性和沉积速率，以及优异的应力强度，并且在由此制造的含硅薄膜中，诸如碳、氧和氢的杂质的含量被最小化，从而可以制造具有高纯度、优异的物理和电性质、优异的耐氟化氢性、优异的水蒸气穿透率以及优异的台阶覆盖率的含硅薄膜。
附图说明
图1是说明通过测量实施例1和2中制备的双(氨基甲硅烷基)烷基胺化合物的蒸气压而获得的结果的图。
图2是说明通过对实施例1和2中制备的双(氨基甲硅烷基)烷基胺化合物进行热重分析而得到的结果的图。
图3是说明通过对实施例3至5中制造的氧化硅薄膜的沉积膜进行红外光谱分析而获得的结果的图。
图4是说明通过对实施例6至9中制造的氮化硅薄膜的沉积膜进行红外光谱分析而获得的结果的图。
具体实施方式
本发明提供了用于沉积含硅薄膜的含有双(氨基甲硅烷基)烷基胺化合物的组合物，该组合物在室温下为液体，并具有高挥发性和优异的热稳定性，因此可用作形成含硅薄膜的有用的前体，其中双(氨基甲硅烷基)烷基胺化合物由以下化学式1表示。
[化学式1]
(在化学式1中，
R是(C1-C7)烷基或(C2-C7)烯基；
R1至R4各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基，或R1和R2以及R3和R4各自独立地相互连接形成环；以及
R5至R8各自独立地为氢、卤素、(C1-C7)烷基或(C2-C7)烯基。)
根据本发明的用于沉积含硅薄膜的组合物含有由化学式1表示的用于沉积薄膜的前体，使得可以在低温下进行成膜，并且同时，可以容易地制造具有高耐久性的高质量薄膜。
此外，根据本发明的用于沉积含硅薄膜的组合物包含由化学式1表示的用于沉积薄膜的前体，该薄膜可以以高薄膜沉积速率沉积，并且该膜具有优异的应力性质和水蒸气穿透率。
原因可能是由于用于沉积含硅薄膜的组合物中包含的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物具有两个氨基甲硅烷基基团和一个烷基或烯基基团作为取代基，所以双(氨基甲硅烷基)烷基胺化合物具有高挥发性和优异的热稳定性。
优选地，在根据示例性实施方式的化学式1中，R5至R7可各自独立地为氢、卤素、(C1-C7)烷基或(C2-C7)烯基，以及R8可为氢。
优选地，根据本发明示例性实施方式的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物可以由以下化学式2或3表示。
[化学式2]
[化学式3]
(在化学式2或3中，
R是(C1-C7)烷基或(C2-C7)烯基；
R5至R7各自独立地为氢、卤素、(C1-C7)烷基或(C2-C7)烯基；
R11至R14各自独立地为氢、(C1-C5)烷基或(C2-C5)烯基；以及
n和m各自独立地为1至7的整数。)
在根据本发明由化学式2或3表示的双(氨基甲硅烷基)烷基胺化合物中，两个氨基甲硅烷基官能团和一个烷基或烯基基团被取代，使得双(氨基甲硅烷基)烷基胺化合物是热稳定的，并且同时，双(氨基甲硅烷基)烷基胺化合物具有硅氮烷主链，其中两个氨基甲硅烷基官能团中的至少一个中的至少一个氢原子被取代，使得双(氨基甲硅烷基)烷基胺化合物在室温下作为液体具有高挥发性。因此，双(氨基甲硅烷基)烷基胺化合物可以非常有用地用于形成含硅薄膜。
更具体地，根据本发明的双(氨基甲硅烷基)烷基胺化合物，其是具有硅氮烷主链的化合物，基本上具有两个氨基甲硅烷基官能团(和或和)，并且氨基甲硅烷基官能团之一中的甲硅烷基必须具有含有至少一个氢原子的官能团(或)，使得双(氨基甲硅烷基)烷基胺化合物作为用于沉积薄膜的前体可以具有优异的效果。
优选地，在根据本发明示例性实施方式的化学式2或3中，R5至R7可各自独立地为氢或(C1-C5)烷基；R11至R14可各自独立地为氢、(C1-C5)烷基或(C2-C5)烯基；以及，n和m可各自独立地为1至4的整数。
更优选地，根据本发明由化学式1表示的双(氨基甲硅烷基)烷基胺化合物可以由以下化学式4或5表示。
[化学式4]
[化学式5]
(在化学式4和5中，
R是(C1-C7)烷基或(C2-C7)烯基；
R11至R14各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基；以及
R5和R6各自独立地为(C1-C7)烷基或(C2-C7)烯基；以及
n和m各自独立地为1至7的整数。)
优选地，在根据本发明示例性实施方式的化学式4和5中，R可以是(C1-C5)烷基；R5和R6可以各自独立地为(C1-C5)烷基；以及，n和m可以各自独立地为1至4的整数。更优选地，双(氨基甲硅烷基)烷基胺化合物可以由化学式4表示，并且在化学式4中，R可以是(C1-C3)烷基；且R5和R6可以各自独立地为(C1-C3)烷基。
优选地，根据本发明示例性实施方式的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物可以由以下化学式6或7表示。
[化学式6]
[化学式7]
(在化学式6和7中，
R是(C1-C7)烷基或(C2-C7)烯基；
R11至R14各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基；以及
n和m各自独立地为1至7的整数。)
更优选地，在化学式6和7中，R可以是(C1-C5)烷基；R11至R14可各自独立地为氢、(C1-C5)烷基或(C2-C5)烯基；n和m可各自独立地为1至4的整数。优选地，R可以为(C1-C5)烷基；R11至R14可各自独立地为(C1-C5)烷基；以及n和m可各自独立地为1至4。更优选地，双(氨基甲硅烷基)烷基胺化合物可以由化学式6表示，其中，在化学式6中，R可以是(C1-C3)烷基；且R11至R14可各自独立地为(C1-C3)烷基。
当根据本发明的双(氨基甲硅烷基)烷基胺化合物的硅氮烷主链中的两个氨基甲硅烷基基团的甲硅烷基基团具有两个或四个氢原子时，双(氨基甲硅烷基)烷基胺化合物作为用于沉积薄膜的前体具有更优异的反应性和热稳定性，使得可以制造更高质量的薄膜。
考虑到用于沉积具有更优异性能的薄膜的前体，根据本发明示例性实施方式的由化学式4表示的双(氨基甲硅烷基)烷基胺化合物可以由以下化学式4-1表示。
[化学式4-1]
(在化学式4-1中，
R是(C1-C7)烷基或(C2-C7)烯基；
R1和R2各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基，或R1和R2各自独立地相互连接形成环；以及
R5是(C1-C7)烷基或(C2-C7)烯基。)
考虑到用于沉积具有更优异性能的薄膜的前体，根据本发明示例性实施方式的由化学式6表示的双(氨基甲硅烷基)烷基胺化合物可以由以下化学式6-1表示。
[化学式6-1]
(在化学式6-1中，
R是(C1-C7)烷基或(C2-C7)烯基；以及
R1和R2各自独立地为(C1-C7)烷基或(C2-C7)烯基，或相互连接形成环。)
根据本发明示例性实施方式的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物的具体实例可包括但不限于以下化合物。
根据本发明的用于沉积含硅薄膜的组合物必须含有作为用于沉积薄膜的前体的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物，并且该双(氨基甲硅烷基)烷基胺化合物可以以在一定范围内的含量包含在用于沉积含硅薄膜的组合物中，其中该含量可以被本领域技术人员根据薄膜的成膜条件、厚度、性质等来确定。
如本文所用，术语“烷基”是指具有1至7个碳原子，优选1至5个碳原子，更优选1至3个碳原子的直链、支链和环状饱和和不饱和烃，并且其实例可包括甲基、乙基、丙基、异丙基、丁基、异丁基、新丁基、戊基等。
如本文所用，术语“卤素”是指卤族元素，并且其实例包括氟、氯、溴和碘。
如本文所用，术语“烯基”作为单一基团或另一基团的一部分是指具有2至7个碳原子和一个或多个碳-碳双键的直链、支链或环状烃基。更优选的烯基是具有2至5个碳原子的低级烯基。最优选的低级烯基是具有约2至3个碳原子的低级烯基。此外，烯基基团可以在随机可用的附连点处被取代。烯基的实例包括乙烯基、丙烯基、烯丙基、丁烯基和4-甲基丁烯基。术语“烯基”和“低级烯基”包括具有顺式和反式取向的基，或者替代地，具有E和Z取向的基。
如本文所用，短语“R1和R2以及R3和R4各自独立地相互连接形成环”包括R1和R2相互连接形成环但R3和R4不形成环的情况；与之相反，R1和R2不形成环而R3和R4相互连接形成环的情况；以及R1和R2相互连接形成环且R3和R4相互连接形成环的情况，其中所形成的环可以是包含N的脂环或芳香环，且优选脂环。
如本文所用，术语“脂环”是指在具有环状键合结构的有机化合物中不是芳族化合物的化合物。
根据本发明的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物可以使用方法制备，只要该方法可以被本领域技术人员公认。
此外，本发明提供了使用根据本发明的用于沉积含硅薄膜的组合物制造含硅薄膜的方法。
由于在制造含硅薄膜的方法中，根据本发明的用于沉积含硅薄膜的组合物含有由化学式1表示的双(氨基甲硅烷基)烷基胺化合物，其在室温和常压下是液体并且具有高挥发性和优异的热稳定性，作为前体被使用，因此可以容易处理，可以制造各种薄膜，并且即使在低温和低功率下，也可以以高沉积速率制造具有高纯度、优异的水蒸气穿透率以及优异的薄膜应力性质的含硅薄膜。
通过根据本发明的方法制造的含硅薄膜具有优异的耐久性和电性质，并且其耐氟化氢性和台阶覆盖率也是优异的。
在根据本发明的制造含硅薄膜的方法中，含硅薄膜可以通过任何方法形成，只要该方法可以被本领域技术人员公认。然而，优选地，含硅薄膜可以通过原子层沉积(ALD)方法、化学气相沉积(CVD)方法、金属有机化学气相沉积(MOCVD)方法、低压化学气相沉积(LPCVD)方法、等离子体增强化学气相沉积(PECVD)方法或等离子体增强原子层沉积(PEALD)方法来形成，但更优选PECVD、ALD或PEALD以使薄膜更容易沉积，并使制造的薄膜具有优异的性能。
根据本发明的含硅薄膜可以是氧化硅(SiO2)膜、碳氧化硅(SiOC)膜、氮化硅(SiN)膜、氮氧化硅(SiON)膜、碳氮化硅(SiCN)膜或碳化硅(SiC)膜，且可以制造具有高质量的各种薄膜，特别是可用作有机发光二极管(OLED)的密封剂的薄膜。
更具体地，根据本发明的制造含硅薄膜的方法可以包括：
a)将安装在腔室中的基底的温度保持在30至500℃；
b)使根据本发明的用于沉积含硅薄膜的组合物与基底接触，以将用于沉积含硅薄膜的组合物吸附在基底中；以及
c)将反应气体注入至其中吸附了用于沉积含硅薄膜的组合物的基底以形成含硅薄膜。
更具体地，根据本发明的制造含硅薄膜的方法可以包括：
A)将安装在腔室中的基底的温度保持在30至500℃；
B)使根据本发明的用于沉积含硅薄膜的组合物与基底接触，以将用于沉积含硅薄膜的组合物吸附在基底中；
C)吹扫剩余的用于沉积含硅薄膜的组合物和副产物；
D)将反应气体注入至其中吸附了用于沉积含硅薄膜的组合物的基底以形成含硅薄膜；以及
E)吹扫剩余的反应气体和副产物，其中步骤D)中的反应气体可以除去用于沉积含硅薄膜的组合物中包含的双(氨基甲硅烷基)烷基胺化合物的配体以形成Si-O原子层。
优选地，根据本发明示例性实施方式的反应气体可以在通过产生等离子体功率为50至1000W的等离子体而激活之后供应。
在根据本发明示例性实施方式的制造含硅薄膜的方法中，使用根据本发明的双(氨基甲硅烷基)烷基胺化合物作为前体，使得反应气体可以优选在30至500℃下，更优选30至300℃下，通过产生50至1000W，优选100至800W，更优选400至600W的低等离子体功率的等离子体来激活，从而可以制造薄膜。
在根据本发明示例性实施方式的制造含硅薄膜的方法中，可以根据所需薄膜的结构或热性质来调节沉积条件。根据本发明示例性实施方式的沉积条件的实例可包括含有双(氨基甲硅烷基)烷基胺化合物的用于沉积含硅薄膜的组合物的注入流速、反应气体和载气的注入流速、压力、RF功率、基底的温度等。作为沉积条件的非限制性实例，用于沉积含硅薄膜的组合物的注入流速可以在10至1000cc/min的范围内调节，载气的注入流速可以在10至1000cc/min的范围内调节，反应气体的注入流速可以在1至1500cc/min的范围内调节，压力可以在0.5至10托的范围内调节，RF功率可以在50至1000W的范围内调节，并且基底的温度可以在30至500℃，优选80至300℃的范围内调节，但是沉积条件不限于此。
在根据本发明的制造含硅薄膜的方法中使用的反应气体不受限制，但可以是选自氢气(H2)、肼(N2H4)、臭氧(O3)、氧气(O2)、氧化亚氮(N2O)氨气(NH3)、氮气(N2)、硅烷(SiH4)、硼烷(BH3)、乙硼烷(B2H6)和磷化氢(PH3)中的一种，或者是其中一种或多种的混合气体，并且载气可以是选自氮气(N2)、氩气(Ar)和氦气(He)中的一种，或者是其中两种或更多种的混合气体。
在根据本发明的制造含硅薄膜的方法中使用的基底可以是包含选自Si、Ge、SiGe、GaP、GaAs、SiC、SiGeC、InAs和InP中的一种或多种半导体材料的基底；绝缘体上硅(SOI)基底；石英基底；用于显示器的玻璃基底；或者由聚酰亚胺、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚甲基丙烯酸甲酯(PMMA)、聚碳酸酯(PC)、聚醚砜(PES)、聚酯等制成的柔性塑料基底，但不限于此。
此外，含硅薄膜可以直接形成在基底上。替代地，也可以在基底和含硅薄膜之间形成大量导电层、介电层、绝缘层等。
此外，本发明提供了能够用作含硅薄膜的前体的双(氨基甲硅烷基)烷基胺化合物。根据本发明的双(氨基甲硅烷基)烷基胺化合物由以下化学式1表示。
(在化学式1中，
R是(C1-C7)烷基或(C2-C7)烯基；以及
R1至R4各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基，或R1和R2以及R3和R4各自独立地相互连接形成环；以及
R5至R8各自独立地为氢、卤素、(C1-C7)烷基或(C2-C7)烯基。)
如上所述，根据本发明的由化学式1表示的双(氨基甲硅烷基)烷基胺化合物在室温下是液体并且具有高挥发性和优异的热稳定性，使得双(氨基甲硅烷基)烷基胺化合物在形成含硅薄膜中用作非常有用的前体。
此外，由于在每个氨基甲硅烷基基团的甲硅烷基(硅)中存在四个氢原子，所以双(氨基甲硅烷基)烷基胺化合物具有优异的反应性，使得薄膜可以以快速沉积速率沉积，并且可以制造具有高纯度的薄膜。
优选地，由化学式1表示的双(氨基甲硅烷基)烷基胺化合物可以由化学式2表示，并且更优选地由化学式6或7表示。
将参考以下实施例详细描述本发明。本说明书和权利要求中使用的术语和词语不应被解释为限于典型含义或字典定义，而应解释为基于一定规则具有与本发明的技术范围相关的含义和概念，根据该规则发明人可以适当地定义该术语的概念，以最恰当地描述他或她知道的用于实施本发明的最佳方法。
因此，在本说明书的实施方式中描述的以及在附图中示出的配置仅指示最优选的实施例而不是指示本发明的所有技术构思，并因此应理解可以存在可以替换上述配置的各种等同物和修改。
此外，在所有以下实施例中，通过本领域已知的等离子体增强原子层沉积(PEALD)方法使用商业化的200mm单晶片淋浴头型ALD装置(CN1，Atomic Premium)进行沉积。另外，通过本领域已知的等离子体增强化学气相沉积(PECVD)方法使用商业化的200mm单晶片淋浴头型CVD(PECVD)装置(CN1，Atomic Premium)进行沉积。
使用椭偏仪(OPTI-PROBE 2600，THERMA-WAVE)测量沉积的含硅薄膜的厚度，并使用红外光谱(IFS66V/S&Hyperion 3000，Bruker Optics)、X-射线光电子能谱、水蒸气穿透率(WVTR)分析仪(MOCON，Aquatran 2)和应力分析仪(Frontier Semiconductor，FSM500TC)分析薄膜的性质。
[实施例1]双(甲基二甲基氨基甲硅烷基)甲胺的制备
在无水和惰性气氛下，将二氯甲基硅烷(SiH(CH3)Cl2，115g(1.0mol))和正戊烷(577g(8mol))放入1000mL火焰干燥烧瓶中，并向其中缓慢加入甲胺(CH3NH2，59g(1.9mol))，同时保持温度在-25℃，之后将混合物搅拌3小时，并通过过滤除去盐酸甲胺((CH3)NH3Cl)。将回收的双(氯甲基甲硅烷基)甲胺((SiH(CH3)Cl)2N(CH3))溶液与正戊烷一起搅拌，并保持温度在-25℃，同时向其中缓慢地加入二甲胺((CH3)2NH，94g(7.13mol))。加入完成之后，将反应溶液缓慢加热至室温并在室温下搅拌6小时。通过过滤所得物除去形成的二甲胺盐酸盐((CH3)2NH2Cl，白色)后，得到滤液。减压下从该滤液中除去溶剂，然后减压蒸馏，从而得到双(甲基二甲基氨基甲硅烷基)甲胺((CH3)2NSiH(CH3))2N(CH3)，71g(0.35mol)，产率：70％)。
1H-NMR(于CDCl3中)：δ0.16(t,6H(Si-CH3)2),2.42(d,3H(NCH3)),2.48(s,12H,((CH3)2NSi))2,4.39(m,2H,(-SiHN)2)。
[实施例2]双(乙基甲基氨基甲硅烷基)甲胺的制备
在无水和惰性气氛下，将二氯硅烷(SiH2Cl2，360g(3.56mol))和正戊烷(3,202g(27.79mol))放入5000mL火焰干燥Sus反应器(高压反应器)中，并向其中缓慢加入甲胺(CH3NH2,210g(6.77mol))，同时保持温度在-25℃，之后将混合物搅拌3小时，并通过过滤除去盐酸甲胺((CH3)NH3Cl)。将回收的双氯甲硅烷基胺((SiH2Cl)2N(CH3))溶液与正戊烷一起搅拌，并保持温度在-25℃，同时向其中缓慢加入乙基甲胺((CH3CH2)(CH3)NH)，421g(7.13mol))。加入完成之后，将反应溶液缓慢加热至室温并在室温下搅拌6小时。通过过滤所得物除去形成的乙基甲胺盐酸盐((CH3CH2)(CH3)NH2Cl),白色)后，得到滤液。减压下从该滤液中除去溶剂，然后减压蒸馏，从而得到双(乙基甲基氨基甲硅烷基)甲胺((CH3CH2)(CH3)NSiH2)2N(CH3)，219g(1.07mol)，收率：60％)。
1H-NMR(于C6D6中)：δ0.97(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)。
[实施例3]使用双(乙基甲基氨基甲硅烷基)甲胺通过PEALD制造氧化硅薄膜
在一般的等离子体增强原子层沉积(PEALD)设备中，使用本领域已知的等离子体增强原子层沉积(PEALD)方法，使用根据本发明的实施例2中制备的双(乙基甲基氨基甲硅烷基)甲胺化合物作为用于形成氧化硅膜的组合物来形成膜。
作为反应气体，氧化亚氮与等离子体一起使用，并且对应于惰性气体的氮气用于吹扫。在0.5秒的反应气体和等离子体时间形成膜。表1中示出了用于沉积氧化硅薄膜的具体方法。
通过分析制造的氧化硅薄膜获得的结果示于表2中，并且通过使用红外光谱法分析沉积的膜获得的结果示于图3中。
[实施例4和5]使用双(乙基甲基氨基甲硅烷基)甲胺通过PEALD制造氧化硅薄膜
除了改变实施例3中的下表1中所示的沉积条件之外，以与实施例3中相同的方式制造氧化硅薄膜，通过分析制造的氧化硅薄膜获得的结果示于下表2中，并且通过使用红外光谱法分析沉积的膜获得的结果在图3中示出。
[表1]通过PEALD的氧化硅薄膜的沉积条件
[表2]氧化硅薄膜的性质评价
[实施例6]使用双(乙基甲基氨基甲硅烷基)甲胺通过PEALD制造氮化硅薄膜
在一般的等离子体增强原子层沉积(PEALD)设备中，使用本领域已知的等离子体增强原子层沉积(PEALD)方法，使用根据本发明的实施例2中制备的双(乙基甲基氨基甲硅烷基)甲胺化合物作为用于形成氮化硅膜的组合物来形成膜。作为反应气体，氮气和氨气与等离子体一起用作第一反应气体，且氮气用作第二反应气体。对应于惰性气体的氮气用于吹扫。表3中示出了用于沉积氮化硅薄膜的具体方法。
通过分析氮化硅薄膜获得的具体结果示于表4中，并且通过使用红外光谱仪分析沉积膜获得的结果示于图4中。
[实施例7至9]使用双(乙基甲基氨基甲硅烷基)甲胺通过PEALD制造氮化硅薄膜
除了改变实施例6中的下表3中所示的条件之外，以与实施例6中相同的方式制造氮化硅薄膜，通过分析制造的氧化硅薄膜获得的结果示于下表4中，并且通过使用红外光谱仪分析沉积的膜获得的结果在图4中示出。
[表3]通过PEALD的氮化硅薄膜的沉积条件
[表4]氮化硅薄膜的性质评价

Claims (16)

1.一种用于沉积含硅薄膜的组合物，所述组合物包含由以下化学式1表示的双(氨基甲硅烷基)烷基胺化合物：
[化学式1]
在化学式1中，
R是C1-C7烷基或C2-C7烯基；
R1至R4各自独立地为氢、C1-C7烷基或C2-C7烯基，或R1和R2以及R3和R4各自独立地相互连接形成环；以及
R5至R8各自独立地为氢、卤素、C1-C7烷基或C2-C7烯基。
2.根据权利要求1所述的组合物，其中，在化学式1中，R5至R7各自独立地为氢、卤素、C1-C7烷基或C2-C7烯基，以及，R8为氢。
3.根据权利要求1所述的组合物，其中，由化学式1表示的所述双(氨基甲硅烷基)烷基胺化合物由以下化学式2或3表示：
[化学式2]
[化学式3]
在化学式2或3中，
R是C1-C7烷基或C2-C7烯基；
R5至R7各自独立地为氢、卤素、C1-C7烷基或C2-C7烯基；
R11至R14各自独立地为氢、C1-C5烷基或C2-C5烯基；以及
n和m各自独立地为1至7的整数。
4.根据权利要求3所述的组合物，其中，在化学式2或3中，R5至R7各自独立地为氢或C1-C7烷基；
R11至R14各自独立地为氢、C1-C5烷基或C2-C5烯基；以及
n和m各自独立地为1至4的整数。
5.根据权利要求1所述的组合物，其中，由化学式1表示的所述双(氨基甲硅烷基)烷基胺化合物由以下化学式4或5表示：
[化学式4]
[化学式5]
在化学式4和5中，
R是C1-C7烷基或C2-C7烯基；
R11至R14各自独立地为氢、C1-C7烷基或C2-C7烯基；
R5和R6各自独立地为C1-C7烷基或C2-C7烯基；以及
n和m各自独立地为1至7的整数。
6.根据权利要求5所述的组合物，其中，在化学式4和5中，R是C1-C5烷基；
R5和R6各自独立地为C1-C5烷基；以及
n和m各自独立地为1至4的整数。
7.根据权利要求1所述的组合物，其中，由化学式1表示的所述双(氨基甲硅烷基)烷基胺化合物由以下化学式6或7表示：
[化学式6]
[化学式7]
在化学式6和7中，
R是C1-C7烷基或C2-C7烯基；
R11至R14各自独立地为氢、C1-C7烷基或C2-C7烯基；以及
n和m各自独立地为1至7的整数。
8.根据权利要求7所述的组合物，其中，在化学式6和7中，R是C1-C5烷基；
R11至R14各自独立地为氢、C1-C5烷基或C2-C5烯基；以及
n和m各自独立地为1至4的整数。
9.根据权利要求1所述的组合物，其中，所述双(氨基甲硅烷基)烷基胺化合物选自以下化合物：
10.一种使用根据权利要求1至9中任一项所述的组合物制造含硅薄膜的方法。
11.根据权利要求10所述的方法，其中，通过原子层沉积方法、化学气相沉积方法、金属有机化学气相沉积方法、低压化学气相沉积方法、等离子体增强化学气相沉积方法或等离子体增强原子层沉积方法进行沉积。
12.根据权利要求10所述的方法，其中，所述含硅薄膜是氧化硅膜、碳氧化硅膜、氮化硅膜、氮氧化硅膜、碳氮化硅膜或碳化硅膜。
13.根据权利要求10所述的方法，包括：
a)将安装在腔室中的基底的温度保持在30至500℃；
b)使根据权利要求1至8中任一项所述的组合物与所述基底接触，以将所述组合物吸附在所述基底中；以及
c)将反应气体注入至其中吸附了所述组合物的所述基底以形成含硅薄膜。
14.根据权利要求13所述的方法，其中，在通过产生等离子体功率为50至1000W的等离子体激活所述反应气体之后，供应所述反应气体。
15.由以下化学式1表示的双(氨基甲硅烷基)烷基胺化合物：
[化学式1]
在化学式1中，
R是C1-C7烷基或C2-C7烯基；
R1至R4各自独立地为氢、C1-C7烷基或C2-C7烯基，或R1和R2以及R3和R4各自独立地相互连接形成环；以及
R5至R8各自独立地为氢、卤素、C1-C7烷基或C2-C7烯基。
16.根据权利要求15所述的双(氨基甲硅烷基)烷基胺化合物，其中，由化学式1表示的所述双(氨基甲硅烷基)烷基胺化合物由化学式2或3表示：
[化学式2]
[化学式3]
在化学式2或3中，
R5至R7各自独立地为氢、卤素、C1-C7烷基或C2-C7烯基；
R11至R14各自独立地为氢、C1-C5烷基或C2-C5烯基；以及
n和m各自独立地为1至7的整数。
CN201880019422.XA 2017-03-29 2018-03-28 沉积含硅薄膜的含双(氨基甲硅烷基)烷基胺化合物的组合物及使用其制造含硅薄膜的方法 Active CN110431204B (zh)

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