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CN101078109A - 从有机氨基硅烷前体制备氧化硅薄膜的方法 - Google Patents

从有机氨基硅烷前体制备氧化硅薄膜的方法 Download PDF

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CN101078109A
CN101078109A CNA2007101042463A CN200710104246A CN101078109A CN 101078109 A CN101078109 A CN 101078109A CN A2007101042463 A CNA2007101042463 A CN A2007101042463A CN 200710104246 A CN200710104246 A CN 200710104246A CN 101078109 A CN101078109 A CN 101078109A
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H·思里丹达姆
萧满超
雷新建
T·R·加夫尼
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Abstract

从有机氨基硅烷前体制备氧化硅薄膜的方法。本发明涉及一种通过CVD在底物上沉积氧化硅层的方法。其中烷基具有至少两个碳原子的有机氨基硅烷前体在氧化剂存在下的反应允许形成氧化硅薄膜。所述的有机氨基硅烷类化合物由上图表示：二异丙基氨基硅烷的用途是形成氧化硅薄膜的优选前体。

Description

从有机氨基硅烷前体制备氧化硅薄膜的方法
                      发明背景
在半导体装置的制造中，化学惰性介电材料例如氧化硅的薄被动层是必需的。氧化硅薄层在多晶硅和金属层之间发挥绝缘体、扩散屏蔽、氧化屏障、沟槽分离、具有高介电击穿电压的金属间介电材料和钝化层的作用。
下列文献和专利被引用作为电子学工业制备氧化硅薄膜所采用的合成沉积方法。
US 5,250,473公开了一种通过低压化学气相淀积(LPCVD)以改进的沉积速度在底物上提供具有基本上均匀的厚度的二氧化硅层的方法。反应物一般包括氧化剂和氯硅烷的混合物，其中氯硅烷是式R2R2SiHCl的一氯硅烷并且其中R2和R2代表烷基。所述的二氧化硅层可以被沉积在不同底物例如铝上。
US 5,382,550公开了在半导体底物上沉积SiO2的CVD方法。一种有机硅化合物例如四乙基正硅酸(TEOS)或二叔丁基硅烷被用作前体。
US 6,391,803公开了一种利用ALD并使用下式的化合物制备氮化硅和氧化硅薄膜的方法：Si[N(CH3)2]4、SiH[N(CH3)2]3、SiH2[N(CH3)2]2或SiH3[N(CH3)2]。三(二甲基氨基)硅烷(TDMAS)优选作为前体。
US 6,153,261公开了一种提高氧化硅、氮化硅和氧氮化硅薄膜的形成中的沉积速度的方法，该方法包括使用二叔丁基氨基硅烷(BTBAS)作为前体反应物。
US 6,974,780公开了一种利用CVD反应器在底物上沉积SiO2薄膜的方法。硅前体，即TEOS、二乙基硅烷、四甲基环四氧基硅氧烷、氟代三乙氧基硅烷和氟代三烷氧基硅烷与水和过氧化氢组合用作反应物。
                      发明简述
本发明涉及一种在底物上沉积氧化硅层的方法。在底物上形成氧化硅层的基本方法中，使硅烷前体与氧化剂在沉积室中于在底物上生成氧化硅层的条件下反应。在本发明所述的方法中用有机氨基硅烷作为硅烷前体。
用作前体的化合物的类型一般用下式表示：
Figure A20071010424600061
其中R和R1选自直链、支链或环状、饱和或不饱和的C2-C10烷基、芳香基、烷基氨基；在式A和式C中的R和R1还可以形成环状基团(CH2)n，其中n是1-6，优选4和5并且R2表示单键、(CH2)n链、环、SiR2，或SiH2。优选的化合物是其中R和R1均是异丙基的式A的化合物。
CVD方法中所用的前体可以提供许多优越性，并且这些优越性包括：
便于在低热条件下形成介电薄膜的能力；
制备具有低酸刻蚀率的薄膜的能力；
通过改变所述前体与含氧源的比例而调节所得氧化硅薄膜中碳含量的能力；
通过改变所述前体与含氮源的比例而调节所得氧化硅薄膜中的氮含量的能力；
克服由于使用不同硅烷前体引起的因沉积速度过快造成的许多生产问题的能力。
                      发明详述
经化学气相淀积法(CVD)和等离子体增强的化学气相淀积法(PECVD)在半导体底物上形成氧化硅薄膜是公知的并且所用沉积方法可以被用于本发明的实践中。在这些方法中排空反应室并将半导体底物置于其中。随后，在其中能够在半导体晶片上形成氧化硅层的条件下将有机硅化合物和氧化源置于反应器室内。这些薄膜还可以在处理过程中通过加入碳、氢和氮源来调整碳、氮和氢的含量(有时是指掺杂量)。通过利用有机氨基硅烷前体制备得到的薄膜常常被称作氧化硅、氧碳化硅、氧氮化硅和碳氧氮化硅薄膜。
一类适用于本发明实践的硅化合物是有机氨基硅烷前体并且它由下式A表示：
Figure A20071010424600071
在此类化合物中，R和R1选自直链、支链或环状、饱和或不饱和的C2-C10烷基、芳香基、烷基氨基、杂环、氢、甲硅烷基，带有或不带有取代基，并且R和R1还可以结合形成环状基团。代表性的取代基是烷基并且特别是C2-4烷基，例如乙基、丙基和丁基，包括其异构体、环状基团例如环丙基、环戊基和环己基。举例说明性的此类中的一些优选化合物用下式表示：
其中n是1-6，优选4和5。
第二类适合用于制备氧化硅层的有机氨基硅烷前体是有机氨基硅烷，其具有两个式B表示的悬垂在一个氮原子上的甲硅烷基。
Figure A20071010424600073
对于A类化合物的R基团，R选自直链、支链或环状、饱和或不饱和的C2-C10烷基、芳香基、烷基氨基和杂环。特定的R基团包括甲基、乙基、丙基、烯丙基、丁基、二甲基氨基以及环状基团例如环丙基、环戊基和环己基。举例的化合物是下式代表的化合物：
Figure A20071010424600081
第三类的氨基硅烷化合物由式C表示。这些一般是其中R和R1与式A中的R和R1相同的二氨基二甲硅烷基化合物。R2基团桥连氮原子。有时R2基团仅仅是介于氮原子之间单键或者可以是桥基，例如SiR2、SiH2、一个链或一个环。结构式如下：
Figure A20071010424600082
具体实例包括下式表示的那些：
Figure A20071010424600083
Figure A20071010424600091
已经发现，虽然上述有机氨基硅烷适合制备半导体底物上的氧化硅薄膜，但是优选的是式A的有机氨基硅烷类化合物。二烷基氨基硅烷类化合物符合一些现有的硅烷类化合物作为前体的标准，原因在于它们形成具有相似介电常数的薄膜。特别是，二异丙基氨基硅烷提供了优良的低刻蚀率，这在工艺中提供了意外的性质，原因在于它是稳定的并且具有比许多其他硅烷前体更长的寿命。
在为化学气相淀积法(CVD)、低压化学气相淀积法(LPCVD)、等离子体增强的CVD(PECVD)、原子层沉积法(ALD)等设计的沉积室内可以形成氧化硅薄膜。在此使用的术语CVD包括半导体工业中采用的各种上述方法。
常规的氧化剂可以用作在沉积室内将二烷基氨基硅烷转化为氧化硅薄膜的氧源。代表性的氧化剂包括过氧化氢、一氧化氮、臭氧和分子氧。通常，氧化剂与硅烷前体的比例大于0.1，优选是每摩尔有机氨基硅烷前体使用0.1-6摩尔氧化剂。
可用于形成氧氮化硅的常用氮源包括氨、肼、烷基肼、二烷基肼及其混合物。
在此所述的式A和B的有机氨基硅烷类化合物给制造者提供了在相对低温下经CVD形成氧化硅薄膜的性能，虽然人们可以在450-600℃的一般温度范围内操作。
低压化学气相淀积方法(LPCVD)涉及允许在多种底物，例如硅和铝上，在一般是0.1-500托，优选0.5-20托的压力范围内发生的化学反应。高压CVD可以在到达所需底物之前产生气相成核作用或者预淀积作用。对于这样的高压反应，可能需要用惰性气体例如氮气和氦气稀释硅烷前体。制造者使用惰性气体达到对前体的相应稀释可以提高淀积的均匀性或者提高对化学蒸气渗透的穿透。
通过使用异丙基氨基硅烷，并且优选二异丙基氨基硅烷作为特定的硅烷前体，可以形成氧化物薄膜，后者以5/分钟-60/分钟的速率沉积并且折射率范围在1.45-1.70，并且湿刻蚀率(在1％HF溶液中)是0.01/秒-1.5/秒。
下列实施例提高本发明的多种举例实施方式并且不限于此范围。
一般性方法
在LPCVD反应器中测试前体用于定量分析氧化硅沉积所用的试验前体。将前体脱气并且经低压质量流控制器(MFC)计量加入到反应器内。根据化学物的重量损失相对于流动时间对MFC流量进行校准。也可以经校准的MFC将附加反应物例如氧和稀释剂例如氮和氦计量加入反应器内。将该反应器与能够排空反应器至低于1E-4托(0.013Pa)的根排风扇/干燥泵的组合连接。在沉积过程中，在整个硅晶片上的温度在设定点的1℃内。
将硅晶片负载在石英船上并且插入反应器中。将反应器泵至基础压力并且检查泄漏。用气流将该体系逐渐调至处理温度，该气流将稀释任何残余的氧或水分以防止硅晶片随着反应器加热而被氧化。随后使反应器稳定持续预定的时间由此使所有硅晶片表面达到相等的温度，该温度是通过上述测量方法在晶片上用所连的热电偶测定的。
在控制的压力下将气体和蒸气注入到反应器内持续预定的沉积时间。其次，关掉气体，并且将反应器泵至基础压力。随后随着反应器被冷却下来，将反应器用泵吹洗，关闭泵，并且用泵吹洗以清除任何反应气体和蒸气。将反应器再次填充至大气压；除去晶片并且冷却至室温。随后测定沉积的薄膜的薄膜厚度、薄膜折射率、薄膜应力、红外吸光率、介电常数和酸刻蚀率。
                       实施例1
         使用二乙基氨基硅烷前体形成氧化硅薄膜
根据上述所列的一般性方法，采用下列反应物和流动条件。使11.7sccm的二乙基氨基硅烷(DEAS)在500℃下与0.6托的5.9sccm O2流入LPCVD反应器中持续74分钟的沉积时间。
氧化硅薄膜的平均薄膜厚度是123nm并且折射率为1.459。该薄膜的湿刻蚀率在1％HF溶液中是1.38/秒。红外光谱中Si-O-Si吸收占优势。C-H吸收在噪音内，指示该薄膜是二氧化硅。卢瑟福反散射能光谱(前向散射的氢)的薄膜组成分析表明此薄膜是28个原子百分数的硅、57个原子百分数的氧、11个原子百分数的氢、3个原子百分数的碳和1个原子百分数的氮，表明此薄膜是含有氢、碳和氮杂质的二氧化硅。
                      实施例2
        使用二乙基氨基硅烷前体形成氧化硅薄膜
采用实施例1的方法，但除了处理条件之外。目的在于测定较高温度和减少的反应时间的影响。在此实施例中，使11.7sccm二乙基氨基硅烷(DEAS)在600℃下与0.6托的5.9sccm O2流入反应器内持续44分钟的沉积时间。
氧化硅的平均薄膜厚度是157nm并且折射率为1.501。该薄膜的湿刻蚀率在1％HF溶液中是0.41/秒。红外光谱中Si-O-Si吸收占优势。C-H吸收在噪音内，指示该薄膜是二氧化硅。卢瑟福反散射能光谱(前向散射的氢)的薄膜组成分析表明此薄膜是27个原子百分数的硅、47个原子百分数的氧、15个原子百分数的氢、7个原子百分数的碳和4个原子百分数的氮，指示此薄膜是含有氢、碳和氮杂质的二氧化硅。
                      实施例3
         使用二异丙基氨基硅烷前体形成氧化硅薄膜
采用实施例1的方法，但除了处理条件和前体之外。在此实施例中，使10.5sccm的二异丙基氨基硅烷(DIPAS)在500℃下与0.6托的5.0sccm O2流入反应器内持续74分钟的沉积时间。
氧化硅的平均薄膜厚度是112nm并且折射率为1.458。该薄膜的湿刻蚀率在1％HF溶液中是1.39/秒。红外光谱中Si-O-Si吸收占优势。C-H吸收在噪音内，指示该薄膜是二氧化硅。卢瑟福反散射能光谱(前向散射的氢)的薄膜组成分析表明此薄膜是28个原子百分数的硅、55个原子百分数的氧、12个原子百分数的氢、3个原子百分数的碳和2个原子百分数的氮，表明此薄膜是含有氢、碳和氮杂质的二氧化硅。
                       实施例4
        使用二异丙基氨基硅烷前体形成氧化硅薄膜
采用实施例2的方法，但除了处理条件和前体之外。在此实施例中，使10.5sccm的二异丙基氨基硅烷(DIPAS)在600℃下与0.6托的5.0sccm O2流入反应器内持续33分钟的沉积时间。
氧化硅的平均薄膜厚度是124nm并且折射率为1.495。该薄膜的湿刻蚀率在1％HF溶液中是0.42/秒。红外光谱中Si-O-Si吸收占优势。C-H吸收在噪音内，指示该薄膜是二氧化硅。卢瑟福反散射能光谱(前向散射的氢)的薄膜组成分析表明此薄膜是28个原子百分数的硅、51个原子百分数的氧、11个原子百分数的氢、6个原子百分数的碳和4个原子百分数的氮，表明此薄膜是含有氢、碳和氮杂质的二氧化硅。
总之，实施例1-4表明，式A表示的类型的有机氨基硅烷可以被用作在半导体底物上制备氧化硅薄膜的前体。二异丙基氨基硅烷DIPAS为用二乙基氨基硅烷(DEAS)在低蚀刻率氧化物方法中作为前体提供了优点。DEAS在室温下不如DIPAS稳定。DEAS的不稳定性可以造成许多EH&S管理、生产、供应线(包括存货和装运)和终端用户过程的挑战。实施例3和4表明，由DIPAS形成的氧化物薄膜一般具有与实施例1和2中在相似处理条件下由DEAS形成的氧化物薄膜相同的刻蚀率、介电常数、折射率和质量组成(经由FTIR)。由此，从化学和工艺的观点看，DIPAS是制备低刻蚀率氧化硅薄膜的优选前体。

Claims (20)

1.一种通过与氧化剂反应经过硅烷氧化物前体的化学气相淀积在底物上形成氧化硅薄膜的方法，该方法包括：
使用选自下式表示的有机氨基硅烷的硅烷前体：
Figure A2007101042460002C1
其中R和R1选自直链、支链或环状、饱和或不饱和的C2-C10烷基、芳香基、烷基氨基；在式A和式C中的R和R1还可以形成环状基团(CH2)n，其中n是1-6，并且R2表示单键、(CH2)n链、环、SiR2或SiH2。
2.权利要求1的方法，其中所述的有机氨基硅烷用式A表示，其中R和R1是具有2-4个碳原子的烷基。
3.权利要求1的方法，其中R和R1是环状的。
4.权利要求1的方法，其中R和R1以(CH2)n的形式结合成环并且其中n是4-5。
5.权利要求2的方法，其中R和R1是异丙基。
6.权利要求1的方法，其中所述的有机氨基硅烷由下式表示：
Figure A2007101042460002C2
并且其中n选自4和5。
7.权利要求1的方法，其中所述的氧化剂选自氧气、过氧化氢、臭氧和一氧化氮。
8.权利要求1的方法，其中所述的有机氨基硅烷由式B表示并且在此类化合物中，所述的有机氨基硅烷选自具有下式的组：
Figure A2007101042460003C1
9.权利要求8的方法，其中所述的氧源选自氧气、过氧化氢、臭氧和一氧化氮。
10.权利要求9的方法，其中所述的有机氨基硅烷用下式表示：
11.权利要求1的方法，其中所述的有机氨基硅烷由式C表示并且在此类化合物中，所述的有机氨基硅烷选自具有下式的组：
Figure A2007101042460003C3
Figure A2007101042460004C1
12.权利要求1的方法，其中碳源和氢源被掺入到沉积室内用于形成掺杂了碳和氢的氧化硅薄膜。
13.权利要求12的方法，其中氮源被掺入到沉积室内用于形成掺杂了碳、氮和氢的氧化硅薄膜。
14.一种通过化学气相淀积法在化学气相淀积室内在底物上制备氧化硅介电层的方法，该方法包括：在使所述的二异丙基氨基硅烷与所述的氧化剂反应的条件下将二异丙基氨基硅烷和氧化剂引入到所述的化学气相淀积室内并且在所述的底物上沉积氧化硅层。
15.权利要求14的方法，其中所述的氧化剂选自臭氧、氧气、一氧化氮和过氧化氢。
16.权利要求15的方法，其中在所述化学气相淀积室内使用350-700℃的温度和0.1-500托的压力。
17.权利要求15的方法，其中氧化剂与二异丙基氨基硅烷的摩尔比是每摩尔二异丙基氨基硅烷使用0.1-10摩尔氧化剂。
18.一种通过化学气相淀积法在化学气相淀积室内在底物上制备氧氮化硅介电层的方法，该方法包括：
在使所述的二异丙基氨基硅烷与所述的氧化剂和所述的氮源反应的条件下将二异丙基氨基硅烷、氮源和氧化剂引入到所述的化学气相淀积室内，从而在所述的底物上沉积氧氮化硅层。
19.权利要求18的方法，其中所述的氧化剂选自臭氧、氧气、一氧化氮和过氧化氢。
20.权利要求18的方法，其中所述的氮源选自氨、肼、烷基肼、二烷基肼及其混合物。
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