CN1522462A - 制备低介电膜的方法 - Google Patents

制备低介电膜的方法 Download PDF

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CN1522462A
CN1522462A CNA02813172XA CN02813172A CN1522462A CN 1522462 A CN1522462 A CN 1522462A CN A02813172X A CNA02813172X A CN A02813172XA CN 02813172 A CN02813172 A CN 02813172A CN 1522462 A CN1522462 A CN 1522462A
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silane
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李时雨
郭相基
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POHANG POLYTECHNIC SCHOOL
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Abstract

本发明通过使用含O2气体等离子体、具有至少一个乙烯基或乙炔基的有机硅或有机硅酸酯化合物，或饱和有机硅或有机硅酸酯化合物和不饱和烃的混合物进行化学气相沉积制备了低介电常数的氢化硅－碳氧化物(SiCO：H)膜。

Description

制备低介电膜的方法
                       技术领域
本发明涉及一种改进的等离子体化学气相沉积(CVD)方法，其用于制备低介电常数的氢化硅-碳氧化物(SiCO:H)膜。
                       背景技术
随着ULSI(超大规模集成)电路中使用的电子器件的尺寸不断减小，出现了层内和/或层间电容增大的问题，从而引起信号延迟。因此，需要开发一种低介电常数(k)的材料，其k值低于常规的二氧化硅(SiO2)或氟氧化硅(SiOF)。
US专利No.6,147,009公开了通过使含有Si、C、O和H原子的前体蒸气在平行板等离子体增强化学气相沉积室中发生反应而制得的一种低介电常数的材料。所述前体是具有环状结构的分子例如1，3，5，7-四甲基环四硅氧烷(TMCTS，C4H16O4Si4)、四乙基环四硅氧烷(C8H24O4Si4)或十甲基环五硅氧烷(C10H30O5Si5)，其中有或没有氧加入。然而，该专利公开的膜的介电常数仍然较高(为3.3至4.0)。为了进一步减小该专利中所述的材料的介电常数，US专利No.6,312,793建议了一种包括两相或多相的低k材料。然而，这种多相材料的K值仍然大于3.2。
因此，本发明人努力开发了一种介电常数比常规材料低的新型材料。
                      发明概述
因此，本发明的一个目的是提供一种使用化学气相沉积(CVD)技术制备改进的低介电常数氢化硅-碳氧化物(SiCO:H)膜的方法。
本发明的另一个目的是提供一种介电常数(k)低于常规低介电材料的SiCOH膜。
根据本发明的一个方面，提供了一种用于制备低介电常数氢化硅-碳氧化物(SiCO:H)膜的方法，其包括与含O2气体等离子体一起，使用具有至少一个乙烯基或乙炔基的有机硅或有机硅酸酯化合物，或饱和有机硅或有机硅酸酯化合物和不饱和烃的混合物进行化学气相沉积。
根据本发明的另一个方面，提供了一种通过所述方法制备的低介电常数的SiCOH薄膜，其介电常数(k)为2.6或更低。
                       附图简介
本发明的上述及其它目的和特征从以下描述并结合附图理解可显而易见，所述附图分别表示为：
图1a和1b：用于形成本发明的薄膜的等离子体反应器的示意图；
图2：本发明的实施例1中得到的膜的碳含量分别随O2/VTMS流量比的变化；
图3：本发明的实施例1和对比实施例1中得到的膜的介电常数分别随O2/VTMS和O2/4MS流量比的变化；
图4和5：实施例1中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化；
图6和7：本发明的实施例2中得到的膜的碳含量和介电常数分别随O2/(4MS+C2F4)流量比的变化；
图8和9：实施例2中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化；
图10：本发明的实施例3中得到的膜的碳含量分别随O2/TVTMCTSO流量比的变化；
图11：本发明的实施例3和对比实施例2中得到的膜的介电常数分别随O2/TVTMCTSO和O2/TMCTSO流量比的变化；
图12和13：实施例3中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化；
图14和15：本发明的实施例4中得到的膜的碳含量和介电常数分别随O2/(TMCTSO+C2H4)流量比的变化；
图16和17：实施例4中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化；
图18和19：本发明的实施例5中得到的膜的碳含量和介电常数分别随O2/DADMS流量比的变化；
图20和21：实施例5中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化；
图22和23：本发明的实施例6中得到的膜的碳含量和介电常数分别随O2/DVTMDSO流量比的变化；
图24和25：实施例6中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化；
图26和27：本发明的实施例7中得到的膜的碳含量和介电常数分别随O2/VTMOS流量比的变化；
图28和29：实施例7中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化；
图30和31：本发明的实施例8中得到的膜的碳含量和介电常数分别随O2/ETMS流量比的变化；
图32和33：本发明的实施例8中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化；
图34和35：本发明的实施例9中得到的膜的碳含量和介电常数分别随O2/(HMDSO+C2H4)流量比的变化；和
图36和37：本发明的实施例9中得到的膜的介电常数分别作为退火温度和退火时间的函数的变化。
                       发明详述
本发明提供了一种用于制备低介电常数氢化硅-碳氧化物(SiCO:H)膜的方法，通过与含O2气体等离子体一起，使用具有至少一个乙烯基或乙炔基的有机硅或有机硅酸酯化合物，或饱和有机硅或有机硅酸酯化合物和不饱和烃的混合物进行化学气相沉积。
根据本发明，可以使用等离子体CVD设备实施(例如遥控等离子体CVD或直接等离子体(direct plasma)CVD设备)来制备低介电常数的SiCOH膜的方法。
图1a所示的遥控等离子体CVD设备包括石英管(6)、天线(9)、匹配器(5)、高频电源(10)、用于硅前体进料的质量流量控制器(7)、前体容器(2)和用于反应气体进料的质量流量控制器(8)。天线缠绕在石英管(6)的外围，由此将天线(9)与匹配器(5)相连接，该匹配器与高频电源(10)相连接。石英管(6)与质量流量控制器(8)连接，该质量流量控制器用于含O2气体经管道的进料。在所述遥控等离子体CVD设备中，含O2气体和硅前体分别被送到匹配器(5)中，前体通过扩散环(3)引入。此外，在图1b所示的直接等离子体CVD设备中，从前体容器(2)供入的硅前体与从反应气体容器(1)供入的含O2气体混合，然后送入匹配器(5)。
根据本发明的一个优选实施方案，提供了一种用于制备低介电常数SiCOH材料的方法，该方法包括使用具有至少一个乙烯基或乙炔基的有机硅或有机硅酸酯化合物和含O2气体等离子体进行化学气相沉积。
含有至少一个乙烯基或乙炔基的不饱和有机硅或有机硅酸酯化合物的典型实例包括乙烯基三甲基硅烷、乙烯基三乙基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、1，3，5-三乙烯基-1，3，5-三甲基环三硅氧烷、1，3，5，7-四乙烯基-1，3，5，7-四甲基环四硅氧烷、1，3-二乙烯基四甲基二硅氧烷、六乙烯基二硅氧烷、烯丙基二甲基硅烷、烯丙基二甲氧基硅烷、乙炔基三甲基硅烷、乙炔基三乙基硅烷以及它们的混合物。
不饱和有机硅或有机硅酸酯化合物可以使用含有一个或多个卤素取代基的有机硅或有机硅酸酯原位(in situ)产生。
根据本发明的另一个优选实施方案，提供了一种用于制备低介电常数SiCOH材料的方法，其包括使用饱和有机硅或有机硅酸酯化合物和不饱和烃的混合物来与含有O2的气体等离子体一起进行化学气相沉积。所述饱和有机硅或有机硅酸酯化合物与所述不饱和烃的混合比优选为1∶0.1至1∶10。如果混合比低于0.1，则膜的介电常数变得过高，而如果混合比超过10，则膜的物理性能变得不能令人满意。
在上述实施方案中，饱和有机硅或有机硅酸酯化合物或不饱和烃可含有一个或多个卤素取代基。
饱和有机硅或有机硅酸酯化合物的典型实例包括三甲基硅烷、三乙基硅烷、三甲氧基硅烷、三乙氧基硅烷、四甲基硅烷、四乙基硅烷、四甲氧基硅烷、四乙氧基硅烷、六甲基环三硅氧烷、四甲基环四硅氧烷、四乙基环四硅氧烷、八甲基环四硅氧烷、六甲基二硅氧烷、双三甲硅烷基甲烷以及它们的混合物。
不饱和烃的典型实例为H2C＝CH2、F2C＝CF2、H2C＝CF2、HFC＝CFH、F2C＝C＝CF2、H2C＝C＝CF2、HFC＝C＝CFH、HC≡CH、FC≡CH、FC≡CF、Cl2C＝CCl2、H2C＝CCl2、HClC＝CClH、Cl2C＝C＝CCl2、H2C＝C＝CCl2、HClC＝C＝CClH、ClC≡CH、ClC≡CCl、Br2C＝CBr2、H2C＝CBr2、HBrC＝CBrH、Br2C＝C＝CBr2、H2C＝C＝CBr2、HBrC＝C＝CBrH、BrC≡CH、BrC≡CBr、I2C＝CI2、H2C＝CI2、HIC＝CIH、I2C＝C＝CI2、H2C＝C＝CI2、HIC＝C＝CIH、IC≡CH和IC≡CI；优选为H2C＝CH2或F2C＝CF2。
可用于本发明的含O2气体选自O2、N2O、O3、H2O2、CO2、H2O以及它们的混合物。
本发明的方法可进一步包括将沉积膜退火的步骤，其可在100至800℃进行0.5至8小时，优选在450℃进行1小时，从而得到热稳定的低介电常数的SiCOH膜。退火步骤还可包括快速热处理，其可在100至900℃的温度范围内进行约1分钟，然后进行10秒的尖峰加热(spike-heating)步骤。
根据本发明的方法制备的这种低介电常数SiCOH材料的介电常数(k)为2.8或更低；此外，退火后形成的热稳定的SiCOH膜的介电常数(k)特别低(为1.6至2.6)，该介电常数(k)可通过调节工艺参数进行控制。
本发明用下文提供的实施例进一步描述和说明，然而这并不意味着本发明范围的限制。
                    实施例1
在图1b所示的直接等离子体设备中，使用乙烯基三甲基硅烷(VTMS，SiC5H12)和O2在Pt底基上沉积SiCOH膜。在膜沉积的过程中，O2/VTMS的流量比在1至13.3的范围内变化。反应器中的压力和温度分别为1mmHg和30℃，施加的等离子体功率为60W。由此沉积的膜在氩气氛下在300至500℃的温度下退火，得到低介电常数的膜。
如图2所示，沉积膜和450℃退火的膜的相应碳含量随着O2/VTMS流量比的增加而降低。图3显示在450℃退火的膜的介电常数为1.8至2.4，而没有经过退火的沉积膜的介电常数为2.3至2.8。图4和5显示在O2/VTMS流量比为2时，实施例1中得到的膜的介电常数随着退火温度和退火时间的变化而变化。
                      对比实施例1
使用四甲基硅烷(4MS，SiC4H12)代替VTMS重复实施例1的步骤，得到一个沉积膜。如图3所示，由此得到的膜的介电常数为3.0至3.5，比实施例1中得到的沉积膜的介电常数高。
                     实施例2
重复实施例1的步骤，不同的是使用四甲基硅烷(4MS，SiC4H12)和C2F4的混合物(1∶1)代替VTMS，得到一个沉积膜，随后将其退火。
图6和图7分别显示沉积膜和退火膜的碳含量和介电常数。沉积膜的介电常数为3.0或更低，450℃退火的膜的介电常数为2.5或更低。图8和图9分别显示在O2/(4MS+C2F4)流量比为4时，退火温度(退火时间＝0.5小时)和退火时间(退火温度＝400℃)对膜的介电常数的影响。在300至500℃退火0.5小时的膜的介电常数为2.75或更低。
                  实施例3
重复实施例1的步骤，使用四乙烯基四甲基环四硅氧烷(TVTMCTSO，Si4O4Cl2H24)代替VTMS，得到一个沉积膜，随后将其退火。
图10和图11分别显示沉积膜和退火膜的碳含量和介电常数。沉积膜的介电常数为2.4或更低，在450℃退火的膜的介电常数为2.2或更低。图12和图13分别显示在O2/TVTMCTSO流量比为4时，退火温度(退火时间＝0.5小时)和退火时间(退火温度＝450℃)对膜的介电常数的影响。在300至500℃退火0.5小时的膜的介电常数为2.1或更低。
                 对比实施例2
重复实施例1的步骤，使用四甲基环四硅氧烷(TMCTSO，Si4O4C4H16)代替VTMS，得到一个沉积膜。如图11所示，由此得到的膜的介电常数为2.5至3.3，比实施例3中得到的沉积膜的介电常数高。
                  实施例4
重复实施例1的步骤，不同的是使用四甲基环四硅氧烷(TMCTSO，Si4O4C4H16)和C2H4的混合物(1∶1)代替VTMS，得到一个沉积膜，随后将其退火。
图14和图15分别显示沉积膜和退火膜的碳含量和介电常数。沉积膜的介电常数为2.3或更低，在450℃退火的膜的介电常数为2.2或更低。图16和图17分别显示在(TMCTSO+C2H4)流量比为2时，退火温度(退火时间＝0.5小时)和退火时间(退火温度＝400℃)对膜的介电常数的影响。在300至500℃退火0.5小时的膜的介电常数为2.05或更低。
                  实施例5
重复实施例1的步骤，使用二烯丙基二甲基硅烷(DADMS，SiC8H16)代替VTMS，得到一个沉积膜，随后使其退火。
图18和图19分别显示沉积膜和退过火的膜的碳含量和介电常数。沉积膜的介电常数为2.8或更低，在450℃退过火的膜的介电常数为2.4或更低。图20和图21分别显示在O2/DADMS流量比为4时退火温度(退火时间＝0.5小时)和退火时间(退火温度＝450℃)对膜的介电常数的影响。在300至500℃退火0.5小时的膜的介电常数为2.35或更低。
                  实施例6
重复实施例1的步骤，不同的是使用1，3-二乙烯基四甲基二硅氧烷(DVTMDSO，Si2OC8H18)代替VTMS，得到一个沉积膜，随后将其退火。
图22和图23分别显示沉积膜和退火膜的碳含量和介电常数。沉积膜的介电常数为2.9或更低，在450℃退火的膜的介电常数为2.4或更低。图24和图25分别显示O2/DVTMDSO流量比为2时退火温度(退火时间＝0.5小时)和退火时间(退火温度＝500℃)对膜的介电常数的影响。在300至500℃退火0.5小时的膜的介电常数为2.15或更低。
                  实施例7
重复实施例1的步骤，使用乙烯基三甲氧基硅烷(VTMOS，SiO3C5H12)代替VTMS，得到一个沉积膜，随后将其退火。
图26和图27分别显示沉积膜和退火膜的碳含量和介电常数。沉积膜的介电常数为2.2至2.75，而在450℃退火的膜的介电常数为1.9至2.55。图28和图29分别显示在O2/VTMOS流量比为2时退火温度(退火时间＝0.5小时)和退火时间(退火温度＝450℃)对膜的介电常数的影响。
在300至500℃退火0.5小时的膜的介电常数为2.4或更低。
                      实施例8
重复实施例1的步骤，不同的是使用乙炔基三甲基硅烷(ETMS，SiC5H10)代替VTMS，得到一个沉积膜，随后将其退火。
图30和图31分别显示沉积膜和退火膜的碳含量和介电常数。沉积膜的介电常数为2.65或更低，在450℃退火的膜的介电常数为2.35或更低。图32和图33分别显示在O2/ETMS流量比为4时退火温度(退火时间＝0.5小时)和退火时间(退火温度＝350℃)对膜的介电常数的影响。在300至500℃退火0.5小时的膜的介电常数为2.35或更低。
                       实施例9
重复实施例1的步骤，使用六甲基二硅氧烷(HMDSO，Si2OC6H18)和C2H4(1∶2)的混合物代替VTMS，得到一个沉积膜，随后将其退火。
图34和图35分别显示沉积膜和退火膜的碳含量和介电常数。沉积膜的介电常数为3.0或更低，在450℃退火的膜的介电常数为2.05或更低。图36和图37分别显示O2/(HMDSO+C2H4)流量比为4时退火温度(退火时间＝0.5小时)和退火时间(退火温度＝450℃)对膜的介电常数的影响。在300至500℃退火0.5小时的膜的介电常数为1.7至1.9。
由以上结果可看出的，根据本发明，通过使用含O2的气体等离子体和不饱和有机硅或有机硅酸酯化合物，或饱和有机硅或有机硅酸酯化合物和不饱和烃的混合物，进行CVD来制备低介电常数的SiCOH膜(其具有2.6或更低的介电常数，这比常规的低k-材料的介电常数还要格外更低)。
虽然本发明只对优选实施方案进行了描述和说明，但其中可以进行各种改变和改进而不脱离本发明的本质原理，本发明的范围仅由所附的权利要求书来限定。

Claims (11)

1.一种用于制备低介电常数的氢化硅-碳氧化物(SiCO:H)膜的方法，其包括使用含O2气体等离子体、具有至少一个乙烯基或乙炔基的有机硅或有机硅酸酯化合物，或饱和有机硅或有机硅酸酯化合物和不饱和烃的混合物来进行化学气相沉积。
2.权利要求1的方法，其中所述饱和有机硅或有机硅酸酯化合物与不饱和烃混合物的混合比为1∶0.1至1∶10。
3.权利要求1的方法，其中所述含有至少一个乙烯基或乙炔基的有机硅或有机硅酸酯化合物选自乙烯基三甲基硅烷、乙烯基三乙基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、1，3，5-三乙烯基-1，3，5-三甲基环三硅氧烷、1，3，5，7-四乙烯基-1，3，5，7-四甲基环四硅氧烷、1，3-二乙烯基四甲基二硅氧烷、六乙烯基二硅氧烷、烯丙基二甲基硅烷、烯丙基二甲氧基硅烷、乙炔基三甲基硅烷、乙炔基三乙基硅烷以及它们的混合物。
4.权利要求3的方法，其中所述含有至少一个乙烯基或乙炔基的有机硅或有机硅酸酯化合物选自乙烯基三甲基硅烷、1，3，5，7-四乙烯基-1，3，5，7-四甲基环四硅氧烷、烯丙基二甲基硅烷、1，3-二乙烯基四甲基二硅氧烷、乙烯基三甲氧基硅烷和乙炔基三甲基硅烷。
5.权利要求1的方法，其中所述饱和有机硅或有机硅酸酯化合物选自三甲基硅烷、三乙基硅烷、三甲氧基硅烷、三乙氧基硅烷、四甲基硅烷、四乙基硅烷、四甲氧基硅烷、四乙氧基硅烷、六甲基环三硅氧烷、四甲基环四硅氧烷、四乙基环四硅氧烷、八甲基环四硅氧烷、六甲基二硅氧烷、双三甲基硅烷基甲烷、乙烯基三甲基硅烷、乙烯基三乙基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、1，3，5-三乙烯基-1，3，5-三甲基环三硅氧烷、1，3，5，7-四乙烯基-1，3，5，7-四甲基环四硅氧烷、1，3-二乙烯基四甲基二硅氧烷、六乙烯基二硅氧烷、烯丙基二甲基硅烷、烯丙基二甲氧基硅烷、乙炔基三甲基硅烷、乙炔基三乙基硅烷以及它们的混合物。
6.权利要求5的方法，其中所述饱和有机硅或有机硅酸酯化合物选自四甲基硅烷、六甲基二硅氧烷和四甲基环四硅氧烷。
7.权利要求1的方法，其中所述不饱和烃选自H2C＝CH2、F2C＝CF2、H2C＝CF2、HFC＝CFH、F2C＝C＝CF2、H2C＝C＝CF2、HFC＝C＝CFH、HC CH、FC CH、FC CF、Cl2C＝CCl2、H2C＝CCl2、HClC＝CClH、Cl2C＝C＝CCl2、H2C＝C＝CCl2、HClC＝C＝CClH、ClCCH、ClC CCl、Br2C＝CBr2、H2C＝CBr2、HBrC＝CBrH、Br2C＝C＝CBr2、H2C＝C＝CBr2、HBrC＝C＝CBrH、BrC CH、BrC CBr、I2C＝CI2、H2C＝CI2、HIC＝CIH、I2C＝C＝CI2、H2C＝C＝CI2、HIC＝C＝CIH、IC CH和IC CI。
8.权利要求7的方法，其中所述不饱和烃选自H2C＝CH2或F2C＝CF2。
9.权利要求1的方法，其中所述含O2气体选自O2、N2O、O3、H2O2、CO2、H2O及其混合物。
10.权利要求1的方法，其还包括将所得沉积膜在100至500℃退火0.5至8小时的步骤。
11.采用权利要求1的方法制备的低介电常数氢化硅-碳氧化物(SiCO:H)膜。
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