WO2019037653A1 - 一种制膜方法 - Google Patents

一种制膜方法 Download PDF

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Publication number
WO2019037653A1
WO2019037653A1 PCT/CN2018/100807 CN2018100807W WO2019037653A1 WO 2019037653 A1 WO2019037653 A1 WO 2019037653A1 CN 2018100807 W CN2018100807 W CN 2018100807W WO 2019037653 A1 WO2019037653 A1 WO 2019037653A1
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Prior art keywords
power
sputtering
pulsed
stage
forming method
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English (en)
French (fr)
Inventor
耿波
白志民
王厚工
丁培军
赵晋荣
罗建恒
张超
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Beijing Naura Microelectronics Equipment Co Ltd
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Beijing Naura Microelectronics Equipment Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3485—Sputtering using pulsed power to the target

Definitions

  • the invention belongs to the technical field of semiconductor processing, and in particular relates to a film forming method.
  • the conventional hard mask film has a lower density, and it is required to deposit a thicker thickness when preparing the film, which greatly increases the aspect ratio of the etched deep hole (Via) and increases the subsequent metal conductive layer in the deep hole.
  • the conventional hard mask process film is subjected to compressive stress (compressive stress) after deposition, which may cause deformation or collapse of a narrow copper pattern in the dielectric film. Therefore, only a TiN hard mask that is denser and more stressful (the positive direction is larger, 0 means no stress, negative is compressive stress, positive value is tensile stress) can be adapted to a more advanced integrated circuit process.
  • PVD physical vapor deposition
  • the existing film forming method can adjust the process parameters less, and the adjustment window of the film stress is small, and high density can not be simultaneously achieved under the premise of ensuring process stability and process cost. Sexual, more stressful film deposition.
  • the technical problem to be solved by the present invention is to provide a film forming method for forming a film of high-density tensile stress based on a sputtering process in accordance with the above-mentioned deficiencies in the prior art to satisfy a more advanced integrated circuit process.
  • a film forming method comprising:
  • the first sputtering stage after applying radio frequency power to the target to achieve plasma ignition, simultaneously applying pulsed DC power and RF power to the target; in the second sputtering stage Stop applying RF power to the target or continue to apply pulsed DC power and RF power to the target at the same time.
  • the stress of the film is adjusted by separately adjusting the magnitude of the pulsed DC power used in the first sputtering stage and the magnitude of the pulsed DC power used in the second sputtering stage.
  • the film stress is adjusted by adjusting the magnitude of the RF power.
  • bias power to the wafer during the first sputtering phase and/or the second sputtering phase
  • Adjusting the film stress by adjusting the magnitude of the bias power during the first sputtering phase and/or the second sputtering phase; or
  • the film stress is adjusted by adjusting the magnitude of the bias power and maintaining the magnitude of the bias power constant during the first sputtering phase and/or the second sputtering phase.
  • the film stress is adjusted by adjusting the magnitude of the process gas pressure during the first sputtering phase and/or the second sputtering phase; or
  • the film stress is adjusted by adjusting the magnitude of the process gas pressure and maintaining the magnitude of the process gas pressure constant during the first sputtering stage and/or the second sputtering stage.
  • the duty ratio of the pulsed DC power used in the first sputtering stage is 40% to 80%; and the duty ratio of the pulsed DC power used in the second sputtering stage is 0%. ⁇ 20%.
  • the duty ratio of the pulsed DC power used in the first sputtering stage is 0% when the application of the RF power to the target is stopped, and the duty of the pulsed DC power used in the second sputtering stage is The ratio is 40% to 80%.
  • the duty ratio of the pulsed DC power used in the first sputtering stage is 0% when the pulsed DC power and the RF power are continuously applied to the target, and the pulse is used in the second sputtering stage.
  • the duty cycle of DC power is 0%.
  • the pulsed DC power used in the first sputtering phase is 5 kW ⁇ 10 kW; the pulsed DC power used in the second sputtering stage is 5 kW to 10 kW.
  • the pulsed DC power used in the first sputtering stage is 1 kW to 6 kW;
  • the pulsed DC power used in the shooting stage is from 1 kW to 6 kW.
  • the RF power is 1 kW to 3 kW.
  • the frequency of the radio frequency power is 13.56 MHz, 27 MHz, 40 MHz or 60 MHz.
  • the time of the first sputtering stage is 5 s to 10 s; and the time of the second sputtering stage is 5 s to 10 s.
  • the bias power is from 0 kW to 2 kW.
  • the preheating step before the step of performing the first sputtering phase and the second sputtering phase until the thickness of the film meets the set requirement, the preheating step further comprises:
  • the wafer is heated until the set temperature is reached.
  • the first set pressure is 1 Torr to 2 Torr; and the set temperature is 300 ° C to 400 ° C.
  • the first sputtering stage and the second sputtering stage are performed in the cycle until the thickness of the film meets the setting requirement, and after the pre-heating step, a pressure-control step is further included,
  • the pressure control steps include:
  • the second gas and the third gas are introduced into the reaction chamber, and the gas pressure of the second gas and the third gas is controlled to keep the process gas pressure constant when the second set pressure is reached.
  • the process gas pressure and the stress of the film are adjusted by adjusting a gas flow ratio of the second gas and the third gas.
  • the first gas is argon; the second gas and the third gas are argon and nitrogen, respectively.
  • the second set air pressure is 10 mT to 200 mT.
  • the film forming method provided by the present invention divides the sputtering process into two stages of cyclic processing, and applies pulsed DC power to the target in the first sputtering stage and the second sputtering stage. Further, the density and stress of the film are increased by setting the duty ratio of the pulsed DC power used in the first sputtering stage and the duty ratio of the pulsed DC power used in the second sputtering stage, respectively.
  • the sputtering energy can be increased without increasing the deposition rate of the film, and increasing the sputtering energy can increase the compactness of the film, and appropriately reduce
  • the deposition rate of the film can extend the film process time, increase production stability, and obtain a film with higher stress. Therefore, the film forming method provided by the invention can simultaneously realize high-density and more stress film deposition under the premise of ensuring process stability and process cost, so as to meet the demanding requirements of advanced integrated circuit technology for film performance, It can reduce the cost and process difficulty of more advanced process technology, especially for the preparation of high density TiN film of 14nm Hardmask process.
  • FIG. 1 is a film forming apparatus used in an embodiment of the present invention
  • FIG. 2 is a flow chart of a film forming method according to a first embodiment of the present invention
  • FIG. 3 is a flow chart of a film forming method according to a second embodiment of the present invention.
  • FIG. 4 is a flow chart of a film forming method according to a third embodiment of the present invention.
  • the film forming apparatus includes a reaction chamber 1 in which a target 2 is disposed at the top of the reaction chamber 1, and a susceptor 3 for carrying a wafer is disposed under the target 2.
  • the film forming apparatus further includes a radio frequency power source 4, a direct current power source 5, a matcher 6, a bias power source 7, and a capacitance adjusting device 8.
  • the RF power source 4 and the DC power source 5 are electrically connected to the target 2 via the matching device 6, so that the RF power source 4 and the DC power source 5 can be avoided compared with the RF power source 4 and the DC power source 5 being separately connected to the target material.
  • the susceptor 3 can be selectively electrically coupled to a bias power source 7 and/or a capacitance adjusting device 8 for applying a negative bias voltage to the susceptor 3 and the wafer thereon.
  • the capacitance adjusting device 8 can adjust the particle energy of the wafer surface and the plasma sheath thickness, thereby improving the stress and density of the film.
  • a film forming method includes:
  • the first sputtering stage and the second sputtering stage are cycled until the thickness of the film satisfies the set requirements.
  • pulsed DC power is applied to the target. Further, the density and stress of the thin film are increased by setting the duty ratio A% of the pulsed direct current power used in the first sputtering stage and the duty ratio B% of the pulsed direct current power used in the second sputtering stage, respectively.
  • the duty ratio of the pulsed DC power is different, and the deposition rate of the film is also different.
  • the sputtering energy can be increased while appropriately reducing the deposition rate of the film.
  • the film forming method provided by the embodiment can simultaneously realize high-density and more stress film deposition under the premise of ensuring process stability and process cost, so as to meet the demanding requirements of advanced integrated circuit technology for film performance. At the same time, it can reduce the cost and process difficulty of the more advanced process technology, especially for the preparation of high-density TiN film of 14nm Hardmask process.
  • the duty ratio A% of the pulsed DC power used in the first sputtering stage is 40% to 80%; and the duty ratio B% of the pulsed DC power used in the second sputtering stage is 0% to 20%.
  • the stress of the film can be adjusted by separately adjusting the magnitude of the pulsed DC power used in the first sputtering stage and the magnitude of the pulsed DC power used in the second sputtering stage.
  • the pulsed DC power used in the first sputtering stage is 5 kW to 10 kW; and the pulsed DC power used in the second sputtering stage is 5 kW to 10 kW.
  • the DC power source applies a certain pulsed DC power to the target to achieve plasma ignition.
  • the duty cycle of the pulsed DC power can be 40% to 80%.
  • the duty ratio of the pulsed DC power is 40% to 80%; the time of the first sputtering stage is 5 s to 10 s.
  • the duty ratio of the pulsed DC power is 0% to 20%; and the time of the second sputtering stage is 5s to 10s.
  • bias power is applied to the wafer during the first sputtering phase and/or the second sputtering phase.
  • the film stress is adjusted by adjusting the magnitude of the bias power. Adjusting the bias power allows for a small fine-tuning of the density and stress of the film, which improves the adjustment accuracy.
  • the magnitude of the bias power is from 0 kW to 2 kW.
  • the bias power can also be maintained at a set value during the sputtering process. Specifically, by adjusting the magnitude of the bias power and keeping the magnitude of the bias power constant during the first sputtering phase and/or the second sputtering phase, the same can be achieved for adjusting the film stress.
  • the film stress is adjusted by adjusting the magnitude of the process gas pressure during the first sputtering phase and/or the second sputtering phase. Adjusting the process gas pressure also allows adjustment of the density and stress of the film.
  • the process gas pressure is the pressure of the reaction chamber.
  • the film stress can also be adjusted by adjusting the magnitude of the process gas pressure and keeping the process gas pressure constant during the first sputtering stage and/or the second sputtering stage.
  • the preheating step further comprises:
  • the wafer is heated until the set temperature is reached.
  • the first gas may be argon; the first set pressure is 1 Torr to 2 Torr; the heating temperature is 300 ° C to 400 ° C; and the heating time is 1 min.
  • the preheating step after the wafer is introduced into the reaction chamber, argon gas is introduced into the reaction chamber until the process gas pressure reaches the first set pressure (1T to 2T). Then, the susceptor temperature was set to 300 ° C to 400 ° C, and the susceptor was heated to the wafer for about 1 min.
  • the preheating step can also be completed in the preheating chamber of the film forming apparatus. After the preheating is completed, the wafer reaching the preset temperature is directly introduced into the reaction chamber.
  • the pressure control step comprising:
  • the second gas and the third gas are introduced into the reaction chamber, and the gas pressure of the second gas and the third gas is controlled to keep the process gas pressure constant when the second set pressure is reached.
  • the process gas pressure and the stress of the film are adjusted by adjusting the gas flow ratio of the second gas and the third gas in the first sputtering stage and/or the second sputtering stage.
  • the second gas and the third gas are argon gas and nitrogen gas respectively; and the second set pressure is 10 mT to 200 mT.
  • a film forming method according to a second embodiment of the present invention is different from the first embodiment described above in that different sputtering methods, that is, pulsed DC power + RF power are used for sputtering.
  • different sputtering methods that is, pulsed DC power + RF power are used for sputtering.
  • the film forming method provided by the second embodiment of the present invention includes:
  • the first sputtering stage and the second sputtering stage are cycled until the thickness of the film satisfies the set requirements.
  • the first sputtering stage after applying radio frequency power to the target to achieve plasma ignition, pulsed DC power and RF power are simultaneously applied to the target.
  • the second sputtering phase the application of radio frequency power to the target is stopped.
  • the duty ratio C% of the pulsed DC power used in the first sputtering stage and the duty ratio D% of the pulsed DC power used in the second sputtering stage are respectively set to increase the film. Density and stress.
  • the duty ratio C% of the pulsed DC power is 0%; and the time of the first sputtering phase is 5s to 10s.
  • the duty ratio D% of the pulsed DC power used in the second sputtering stage is 40% to 80%; the time in the second sputtering stage is 5 s to 10 s.
  • the stress of the film can be adjusted by separately adjusting the magnitude of the pulsed DC power used in the first sputtering stage and the magnitude of the pulsed DC power used in the second sputtering stage.
  • the pulsed DC power used in the first sputtering stage is 1 kW to 6 kW; and the pulsed DC power used in the second sputtering stage is 1 kW to 6 kW.
  • the RF power is from 1 kW to 3 kW.
  • the frequency of the RF power is 13.56 MHz, 27 MHz, 40 MHz or 60 MHz.
  • the bias power is applied to the wafer during the first sputtering phase and/or the second sputtering phase. Also, during the sputtering process, the film stress is adjusted by adjusting the magnitude of the bias power. Alternatively, the bias power can be maintained at a set value during sputtering.
  • the film stress is adjusted by adjusting the magnitude of the process gas pressure during the first sputtering phase and/or the second sputtering phase.
  • the film stress can also be adjusted by adjusting the magnitude of the process gas pressure and maintaining the magnitude of the process gas pressure constant during the first sputtering stage and/or the second sputtering stage.
  • the first sputtering stage and the second sputtering stage are performed in the above-described cycle, and the preheating step is further included until the thickness of the film satisfies the setting requirement.
  • the preheating step has been described in detail in the above first embodiment, and will not be described herein.
  • a pressure control step is further included.
  • the pressure control step has been described in detail in the above first embodiment, and details are not described herein again.
  • a film forming method according to a third embodiment of the present invention is different from the second embodiment described above in that both the first sputtering stage and the second sputtering stage simultaneously apply pulsed direct current to the target. Power and RF power.
  • the film forming method provided by the third embodiment of the present invention includes:
  • the first sputtering stage and the second sputtering stage are cycled until the thickness of the film satisfies the set requirements.
  • pulsed DC power and RF power are simultaneously applied to the target.
  • simultaneous application of pulsed DC power and RF power to the target continues.
  • the duty ratio E% of the pulsed DC power used in the first sputtering stage and the duty ratio F% of the pulsed DC power used in the second sputtering stage are respectively set to increase the film. Density and stress.
  • the duty ratio E% of the pulsed DC power used in the first sputtering phase is 0%, and the duty of the pulsed DC power used in the second sputtering phase is occupied.
  • the ratio F% is 0%.
  • the stress of the film can be adjusted by separately adjusting the magnitude of the pulsed DC power used in the first sputtering stage and the magnitude of the pulsed DC power used in the second sputtering stage.
  • the pulsed DC power used in the first sputtering stage is 1 kW to 6 kW; and the pulsed DC power used in the second sputtering stage is 1 kW to 6 kW.
  • the RF power is from 1 kW to 3 kW.
  • the frequency of the RF power is 13.56 MHz, 27 MHz, 40 MHz or 60 MHz.
  • the bias power is applied to the wafer during the first sputtering phase and/or the second sputtering phase. Also, during the sputtering process, the film stress is adjusted by adjusting the magnitude of the bias power. Alternatively, the bias power can be maintained at a set value during sputtering.
  • the film stress is adjusted by adjusting the magnitude of the process gas pressure in the first sputtering stage and/or the second sputtering stage.
  • the film stress can also be adjusted by adjusting the size of the process gas pressure and maintaining the magnitude of the process gas pressure constant during the first sputtering stage and/or the second sputtering stage.
  • the first sputtering stage and the second sputtering stage are performed in the above-described cycle, and the preheating step is further included until the thickness of the film satisfies the setting requirement.
  • the preheating step has been described in detail in the above first and second embodiments, and details are not described herein again.
  • a pressure control step is further included.
  • the pressure control step has been described in detail in the above first and second embodiments, and details are not described herein again.
  • the film data obtained by the film forming methods provided by the first to third embodiments are compared with the film data obtained by the film forming method of the prior art.
  • the conventional film forming method employs a single-step sputtering method and applies pulsed DC power to the target.
  • the film obtained by this method has a density of 4.5 to 4.9 g/cc and a low density.
  • the film has a stress of ⁇ 0, which is a compressive stress and cannot be adapted to a more advanced integrated circuit process.
  • the film obtained by the film forming method provided by the first to third embodiments of the present invention has a density of more than 5.0 g/cc, and a hard mask having a tensile stress of 100 to 1000 MPa can be obtained.

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Abstract

一种制膜方法，包括循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求；其中，在第一溅射阶段和第二溅射阶段中，向靶材施加脉冲直流功率；并且，通过分别设定第一溅射阶段采用的脉冲直流功率的占空比和第二溅射阶段采用的脉冲直流功率的占空比，来提高薄膜的密度和应力。制膜方法可以在保证工艺稳定性和工艺成本的前提下，同时实现高致密性、更大应力的薄膜沉积。

Description

一种制膜方法 技术领域
本发明属于半导体加工技术领域，具体涉及一种制膜方法。
背景技术
近年来，随着集成电路的大规模发展，芯片关键尺寸不断缩小，铜互连制造工艺面临的挑战越来越多。为了保证16nm以下及更小的铜互连结构的紧凑以及结构的完整性，需要更加先进的硬掩膜技术。在更加先进的工艺制造流程中，硬掩膜技术(Hardmask)主要作用是保持较软的超低k电介质材料中的铜线和通孔的图形完整性。然而随着芯片制程尺寸的不断缩小，传统的硬掩膜层(如TiN层)因存在多种问题而无法适用于更先进的集成电路工艺制程。一方面，传统的硬掩膜薄膜密度较低，在制备薄膜时需要沉积较厚的厚度，这就大大增加了蚀刻深孔(Via)的深宽比，且增加了后续金属导电层在深孔中的填充等一系列工艺的难度。另一方面，传统的硬掩膜工艺薄膜沉积后均为压缩应力(Compress，即压应力)，这可能会导致电介质薄膜中狭窄的铜线图案发生变形或者倒塌。因此，只有制备更加致密，且应力更大(正值越大方向，0表示没有应力，负值为压应力，正值为张应力)的TiN硬掩膜，才能适应更先进的集成电路制程。
在集成电路制造工艺中，物理气相沉积(PVD)方式被广泛应用于沉积许多种不同的金属层、硬掩膜等相关材料层。但是，利用上述传统的溅射设备，现有的制膜方法可调整的工艺参数较少，对薄膜应力的调整窗口较小，在保证工艺稳定性和工艺成本的前提下，无法同时实现高致密性、更大应力的薄膜沉积。
发明内容
本发明所要解决的技术问题是针对现有技术中上述不足，提供一种制膜方法，基于溅射工艺形成高密度张应力的薄膜的制备，以满足更加先进的集成电路工艺。
为实现本发明的目的而提供一种制膜方法，其包括：
循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求；
其中，在所述第一溅射阶段和第二溅射阶段中，向靶材施加脉冲直流功率；
并且，通过分别设定所述第一溅射阶段采用的所述脉冲直流功率的占空比和所述第二溅射阶段采用的所述脉冲直流功率的占空比，来提高薄膜的密度和应力。
可选的，在所述第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率；在所述第二溅射阶段中，停止向靶材施加射频功率或者继续同时向靶材施加脉冲直流功率和射频功率。
可选的，通过分别调节所述第一溅射阶段采用的所述脉冲直流功率的大小和所述第二溅射阶段采用的所述脉冲直流功率的大小，来调节薄膜的应力。
可选的，在所述第一溅射阶段中，通过调节所述射频功率的大小，来调节薄膜应力。
可选的，在所述第一溅射阶段和/或第二溅射阶段中，向晶圆加载偏压功率；
通过在进行所述第一溅射阶段和/或第二溅射阶段的过程中调节所述偏压功率的大小，来调节薄膜应力；或者，
通过调节所述偏压功率的大小，并在所述第一溅射阶段和/或第二溅射阶 段中保持所述偏压功率的大小恒定，来调节薄膜应力。
可选的，通过在进行所述第一溅射阶段和/或第二溅射阶段的过程中调节工艺气压的大小，来调节薄膜应力；或者，
通过调节所述工艺气压的大小，并在所述第一溅射阶段和/或第二溅射阶段中保持所述工艺气压的大小恒定，来调节薄膜应力。
可选的，所述第一溅射阶段采用的所述脉冲直流功率的占空比为40％～80％；所述第二溅射阶段采用的所述脉冲直流功率的占空比为0％～20％。
可选的，当在所述第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率；在所述第二溅射阶段中，停止向靶材施加射频功率时，所述第一溅射阶段采用的所述脉冲直流功率的占空比为0％，所述第二溅射阶段采用的所述脉冲直流功率的占空比为40％～80％。
可选的，当在所述第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率；在所述第二溅射阶段中，继续同时向靶材施加脉冲直流功率和射频功率时，所述第一溅射阶段采用的所述脉冲直流功率的占空比为0％，所述第二溅射阶段采用的所述脉冲直流功率的占空比为0％。
可选的，当在所述第一溅射阶段和第二溅射阶段中，仅向靶材施加脉冲直流功率时，所述第一溅射阶段采用的所述脉冲直流功率的大小为5kW～10kW；所述第二溅射阶段采用的所述脉冲直流功率的大小为5kW～10kW。
可选的，当在所述第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率；在所述第二溅射阶段中，停止向靶材施加射频功率或者继续同时向靶材施加脉冲直流功率和射频功率时，所述第一溅射阶段采用的所述脉冲直流功率的大小为1kW～6kW；所述第二溅射阶段采用的所述脉冲直流功率的大小为1kW～6kW。
可选的，所述射频功率的大小为1kW～3kW。
可选的，所述射频功率的频率为13.56MHz、27MHz、40MHz或60MHz。
可选的，所述第一溅射阶段的时间为5s～10s；所述第二溅射阶段的时间为5s～10s。
可选的，所述偏压功率的大小为0kW～2kW。
可选的，在所述循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求的步骤之前，还包括预加热步骤，所述预加热步骤包括：
向反应腔室通入第一气体，直至工艺气压达到第一设定气压；
对晶圆进行加热，直至达到设定温度。
可选的，所述第一设定气压为1Torr～2Torr；所述设定温度为300℃～400℃。
可选的，在所述循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求的步骤之前，且在所述预加热步骤之后，还包括控压步骤，所述控压步骤包括：
对所述反应腔室进行抽气；
同时向所述反应腔室通入第二气体和第三气体，并通过控制所述第二气体和第三气体的气体流量，来使工艺气压在达到第二设定气压时保持恒定。
可选的，在所述第一溅射阶段和/或第二溅射阶段中，通过调节所述第二气体和第三气体的气体流量比，来调节工艺气压和薄膜的应力。
可选的，所述第一气体为氩气；第二气体和第三气体分别为氩气和氮气。
可选的，所述第二设定气压为10mT～200mT。
本发明的有益效果是：
本发明提供的制膜方法，其溅射过程分为循环进行的两个阶段，且在第一溅射阶段和第二溅射阶段中，向靶材施加脉冲直流功率。并且，通过分别设定第一溅射阶段采用的脉冲直流功率的占空比和第二溅射阶段采用的脉冲 直流功率的占空比，来提高薄膜的密度和应力。由此，通过在两个阶段中分别配置相应的脉冲直流功率的占空比，可以增加溅射能量但并不会增加薄膜的沉积速率，增加溅射能量能够提高薄膜的致密性，而适当降低薄膜的沉积速率可以延长薄膜工艺时间，增加生产稳定性，获得应力更大的薄膜。因此，本发明提供的制膜方法，可以在保证工艺稳定性和工艺成本的前提下，同时实现高致密性、更大应力的薄膜沉积，以满足先进集成电路工艺对薄膜性能的苛刻需求，同时可降低更先进制程工艺的成本和工艺方案难度，特别适用于14nm Hardmask工艺的高密度TiN薄膜的制备。
附图说明
图1为本发明实施例采用的制膜设备；
图2为本发明第一实施例提供的制膜方法的流程框图；
图3为本发明第二实施例提供的制膜方法的流程框图；
图4为本发明第三实施例提供的制膜方法的流程框图。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合附图和具体实施方式对本发明提供的制膜方法作进一步详细描述。
图1为本发明实施例采用的制膜设备。请参阅图1，该制膜设备包括反应腔室1，在反应腔室1的顶部设置有靶材2，且在靶材2的下方设置有用于承载晶圆的基座3。制膜设备还包括射频电源4、直流电源5、匹配器6、偏压电源7和电容调节装置8。其中，射频电源4和直流电源5均经由匹配器6与靶材2电连接，这样设置与射频电源4和直流电源5单独与靶材电连接相比，可以避免因射频电源4和直流电源5匹配不佳而引发的打火问题。
在本实施例中，基座3能够可选择的与偏压电源7和/或电容调节装置8电连接，偏压电源7用于向基座3及其上的晶圆加载负偏压。电容调节装置 8能够调节晶圆表面的粒子能量和等离子体鞘层厚度，从而可以改善薄膜的应力和密度。
第一实施例
请参阅图2，本发明第一实施例提供的制膜方法，其包括：
循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求。
其中，在第一溅射阶段和第二溅射阶段中，向靶材施加脉冲直流功率。并且，通过分别设定第一溅射阶段采用的脉冲直流功率的占空比A％和第二溅射阶段采用的脉冲直流功率的占空比B％，来提高薄膜的密度和应力。
脉冲直流功率的占空比不同，薄膜的沉积速率也不同，一般情况，相同工艺条件下，沉积速率越高则薄膜应力趋向压应力(负值越大方向)，而沉积速率越低则应力趋向张应力(正值越大方向，0表示没有应力，负值为压应力，正值为张应力)。基于此，通过分别设定第一溅射阶段采用的脉冲直流功率的占空比和第二溅射阶段采用的脉冲直流功率的占空比，可以增加溅射能量，同时适当降低薄膜的沉积速率，以平衡沉积速率和溅射能量的关系，增加溅射能量能够提高薄膜的致密性，而适当降低薄膜的沉积速率可以延长薄膜工艺时间，增加生产稳定性，获得应力更大的薄膜。
由此，本实施例提供的制膜方法，可以在保证工艺稳定性和工艺成本的前提下，同时实现高致密性、更大应力的薄膜沉积，以满足先进集成电路工艺对薄膜性能的苛刻需求，同时可降低更先进制程工艺的成本和工艺方案难度，特别适用于14nm Hardmask工艺的高密度TiN薄膜的制备。
可选的，第一溅射阶段采用的脉冲直流功率的占空比A％为40％～80％；第二溅射阶段采用的脉冲直流功率的占空比B％为0％～20％。
可选的，可以通过分别调节第一溅射阶段采用的脉冲直流功率的大小和第二溅射阶段采用的脉冲直流功率的大小，来调节薄膜的应力。优选的，第 一溅射阶段采用的脉冲直流功率的大小为5kW～10kW；第二溅射阶段采用的脉冲直流功率的大小为5kW～10kW。
可选的，直流电源向靶材施加一定的脉冲直流功率，以实现等离子体启辉。启辉时，脉冲直流功率的占空比可以为40％～80％。第一溅射阶段，脉冲直流功率的占空比为40％～80％；第一溅射阶段的时间为5s～10s。第二溅射阶段，脉冲直流功率的占空比为0％～20％；第二溅射阶段的时间为5s～10s。
可选的，在第一溅射阶段和/或第二溅射阶段中，向晶圆加载偏压功率。并且，在进行第一溅射阶段和/或第二溅射阶段的过程中，通过调节偏压功率的大小，来调节薄膜应力。调节偏压功率能够对薄膜的密度和应力进行小幅度的微调，从而可以提高调节精度。优选的，偏压功率的大小为0kW～2kW。
需要说明的是，在实际应用中，也可以在溅射过程中将偏压功率保持在设定值。具体地，通过调节偏压功率的大小，并在第一溅射阶段和/或第二溅射阶段中保持偏压功率的大小恒定，这同样可以达到调节薄膜应力的目的。
可选的，在进行第一溅射阶段和/或第二溅射阶段的过程中，通过调节工艺气压的大小，来调节薄膜应力。调节工艺气压也可以对薄膜的密度和应力进行调节。工艺气压即为反应腔室的压强。当然，在实际应用中，也可以通过调节工艺气压的大小，并在第一溅射阶段和/或第二溅射阶段中保持工艺气压的大小恒定，来调节薄膜应力。
可选的，在上述循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求的步骤之前，还包括预加热步骤，该预加热步骤包括：
向反应腔室通入第一气体，直至工艺气压达到第一设定气压；
对晶圆进行加热，直至达到设定温度。
可选的，第一气体可以为氩气；第一设定气压为1Torr～2Torr；加热温度为300℃～400℃；加热时间为1min。
在预加热步骤中，在将晶圆传入反应腔室之后，向反应腔室内通入氩气，直至工艺气压达到第一设定气压(1T～2T)。然后，将基座温度设定为300℃～400℃，使基座对晶圆进行加热约1min。
当然，该预加热步骤也可以在制膜设备的预加热腔室内完成，在完成预加热之后，将达到预设温度的晶圆直接传入反应腔室内。
可选的，在上述预加热步骤之后，还包括控压步骤，该控压步骤包括：
对反应腔室进行抽气；
同时向反应腔室通入第二气体和第三气体，并通过控制第二气体和第三气体的气体流量，来使工艺气压在达到第二设定气压时保持恒定。
可选的，在第一溅射阶段和/或第二溅射阶段中，通过调节第二气体和第三气体的气体流量比，来调节工艺气压和薄膜的应力。
可选的，第二气体和第三气体分别为氩气和氮气；第二设定气压为10mT～200mT。
第二实施例
请参阅图3，本发明第二实施例提供的制膜方法，其与上述第一实施例相比，其区别在于：采用不同的溅射方式，即，脉冲直流功率+射频功率的方式进行溅射。
具体地，本发明第二实施例提供的制膜方法，其包括：
循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求。
其中，在第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率。在第二溅射阶段中，停止向靶材施加射频功率。
与上述第一实施例相类似的，分别设定第一溅射阶段采用的脉冲直流功率的占空比C％和第二溅射阶段采用的脉冲直流功率的占空比D％，以提高 薄膜的密度和应力。
可选的，为了实现脉冲直流功率与高频射频功率的匹配，在第一溅射阶段中，脉冲直流功率的占空比C％为0％；第一溅射阶段的时间为5s～10s。第二溅射阶段采用的脉冲直流功率的占空比D％为40％～80％；第二溅射阶段的时间为5s～10s。
可选的，可以通过分别调节第一溅射阶段采用的脉冲直流功率的大小和第二溅射阶段采用的脉冲直流功率的大小，来调节薄膜的应力。优选的，第一溅射阶段采用的脉冲直流功率的大小为1kW～6kW；第二溅射阶段采用的脉冲直流功率的大小为1kW～6kW。
可选的，射频功率的大小为1kW～3kW。射频功率的频率为13.56MHz、27MHz、40MHz或60MHz。
与上述第一实施例相类似的，在第一溅射阶段和/或第二溅射阶段中，向晶圆加载偏压功率。并且，在溅射过程中，通过调节偏压功率的大小，来调节薄膜应力。或者，也可以在溅射过程中将偏压功率保持在设定值。
与上述第一实施例相类似的，在进行第一溅射阶段和/或第二溅射阶段的过程中，通过调节工艺气压的大小，来调节薄膜应力。或者，也可以通过调节工艺气压的大小，并在第一溅射阶段和/或第二溅射阶段中保持工艺气压的大小恒定，来调节薄膜应力。
与上述第一实施例相类似的，在上述循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求的步骤之前，还包括预加热步骤。该预加热步骤在上述第一实施例中已有了详细描述，在此不再赘述。
可选的，在上述预加热步骤之后，还包括控压步骤。该控压步骤在上述第一实施例中已有了详细描述，在此不再赘述。
第三实施例
请参阅图4，本发明第三实施例提供的制膜方法，其与上述第二实施例 相比，其区别在于：第一溅射阶段和第二溅射阶段均同时向靶材施加脉冲直流功率和射频功率。
具体地，本发明第三实施例提供的制膜方法，其包括：
循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求。
其中，在第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率。在第二溅射阶段中，继续同时向靶材施加脉冲直流功率和射频功率。
与上述第二实施例相类似的，分别设定第一溅射阶段采用的脉冲直流功率的占空比E％和第二溅射阶段采用的脉冲直流功率的占空比F％，以提高薄膜的密度和应力。
可选的，为了实现脉冲直流功率与高频射频功率的匹配，第一溅射阶段采用的脉冲直流功率的占空比E％为0％，第二溅射阶段采用的脉冲直流功率的占空比F％为0％。
可选的，可以通过分别调节第一溅射阶段采用的脉冲直流功率的大小和第二溅射阶段采用的脉冲直流功率的大小，来调节薄膜的应力。优选的，第一溅射阶段采用的脉冲直流功率的大小为1kW～6kW；第二溅射阶段采用的脉冲直流功率的大小为1kW～6kW。
可选的，射频功率的大小为1kW～3kW。射频功率的频率为13.56MHz、27MHz、40MHz或60MHz。
与上述第一、第二实施例相类似的，在第一溅射阶段和/或第二溅射阶段中，向晶圆加载偏压功率。并且，在溅射过程中，通过调节偏压功率的大小，来调节薄膜应力。或者，也可以在溅射过程中将偏压功率保持在设定值。
与上述第一、第二实施例相类似的，在第一溅射阶段和/或第二溅射阶段中，通过调节工艺气压的大小，来调节薄膜应力。或者，也可以通过调节工 艺气压的大小，并在第一溅射阶段和/或第二溅射阶段中保持工艺气压的大小恒定，来调节薄膜应力。
与上述第一、第二实施例相类似的，在上述循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求的步骤之前，还包括预加热步骤。该预加热步骤在上述第一、第二实施例中已有了详细描述，在此不再赘述。
可选的，在上述预加热步骤之后，还包括控压步骤。该控压步骤在上述第一、第二实施例中已有了详细描述，在此不再赘述。
下面对采用第一至第三实施例提供的制膜方法获得的薄膜数据与采用现有技术中制膜方法获得的薄膜数据进行对比。
表1，为第一至第三实施例提供的制膜方法的工艺参数和薄膜数据与现有技术中制膜方法的工艺参数和薄膜数据。
Figure PCTCN2018100807-appb-000001
由上述表1可知，现有技术的制膜方法采用单步溅射方式，且向靶材施加脉冲直流功率。采用这种方法获得的薄膜的密度为4.5～4.9g/cc，密度较低，同时，薄膜的应力＜0，为压应力，无法适应更先进的集成电路制程。与之相比，采用本发明第一至第三实施例提供的制膜方法获得的薄膜的密度超过5.0g/cc，并且可以获得张应力为100～1000MPa的硬掩膜。由此，可以在保 证工艺稳定性和工艺成本的前提下，同时实现高致密性、更大应力的薄膜沉积，以满足先进集成电路工艺对薄膜性能的苛刻需求。
可以理解的是，以上实施方式仅仅是为了说明本发明的原理而采用的示例性实施方式，然而本发明并不局限于此。对于本领域内的普通技术人员而言，在不脱离本发明的精神和实质的情况下，可以做出各种变型和改进，这些变型和改进也视为本发明的保护范围。

Claims (21)

  1. 一种制膜方法，其特征在于，包括：
    循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求；
    其中，在所述第一溅射阶段和第二溅射阶段中，向靶材施加脉冲直流功率；
    并且，通过分别设定所述第一溅射阶段采用的所述脉冲直流功率的占空比和所述第二溅射阶段采用的所述脉冲直流功率的占空比，来提高薄膜的密度和应力。
  2. 根据权利要求1所述的制膜方法，其特征在于，在所述第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率；在所述第二溅射阶段中，停止向靶材施加射频功率或者继续同时向靶材施加脉冲直流功率和射频功率。
  3. 根据权利要求1或2所述的制膜方法，其特征在于，通过分别调节所述第一溅射阶段采用的所述脉冲直流功率的大小和所述第二溅射阶段采用的所述脉冲直流功率的大小，来调节薄膜的应力。
  4. 根据权利要求2所述的制膜方法，其特征在于，在所述第一溅射阶段中，通过调节所述射频功率的大小，来调节薄膜应力。
  5. 根据权利要求1或2所述的制膜方法，其特征在于，在所述第一溅射阶段和/或第二溅射阶段中，向晶圆加载偏压功率；
    通过在进行所述第一溅射阶段和/或第二溅射阶段的过程中调节所述偏压功率的大小，来调节薄膜应力；或者，
    通过调节所述偏压功率的大小，并在所述第一溅射阶段和/或第二溅射阶段中保持所述偏压功率的大小恒定，来调节薄膜应力。
  6. 根据权利要求1或2所述的制膜方法，其特征在于，通过在进行所述第一溅射阶段和/或第二溅射阶段的过程中调节工艺气压的大小，来调节薄膜应力；或者，
    通过调节所述工艺气压的大小，并在所述第一溅射阶段和/或第二溅射阶段中保持所述工艺气压的大小恒定，来调节薄膜应力。
  7. 根据权利要求1所述的制膜方法，其特征在于，所述第一溅射阶段采用的所述脉冲直流功率的占空比为40％～80％；所述第二溅射阶段采用的所述脉冲直流功率的占空比为0％～20％。
  8. 根据权利要求2所述的制膜方法，其特征在于，当在所述第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率；在所述第二溅射阶段中，停止向靶材施加射频功率时，所述第一溅射阶段采用的所述脉冲直流功率的占空比为0％，所述第二溅射阶段采用的所述脉冲直流功率的占空比为40％～80％。
  9. 根据权利要求2所述的制膜方法，其特征在于，当在所述第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率；在所述第二溅射阶段中，继续同时向靶材施加脉冲直流功率和射频功率时，所述第一溅射阶段采用的所述脉冲直流功率的占空比为0％，所述第二溅射阶段采用的所述脉冲直流功率的占空比为0％。
  10. 根据权利要求3所述的制膜方法，其特征在于，当在所述第一溅射阶段和第二溅射阶段中，仅向靶材施加脉冲直流功率时，所述第一溅射阶段 采用的所述脉冲直流功率的大小为5kW～10kW；所述第二溅射阶段采用的所述脉冲直流功率的大小为5kW～10kW。
  11. 根据权利要求3所述的制膜方法，其特征在于，当在所述第一溅射阶段中，在向靶材施加射频功率以实现等离子体启辉之后，同时向靶材施加脉冲直流功率和射频功率；在所述第二溅射阶段中，停止向靶材施加射频功率或者继续同时向靶材施加脉冲直流功率和射频功率时，所述第一溅射阶段采用的所述脉冲直流功率的大小为1kW～6kW；所述第二溅射阶段采用的所述脉冲直流功率的大小为1kW～6kW。
  12. 根据权利要求4所述的制膜方法，其特征在于，所述射频功率的大小为1kW～3kW。
  13. 根据权利要求2所述的制膜方法，其特征在于，所述射频功率的频率为13.56MHz、27MHz、40MHz或60MHz。
  14. 根据权利要求1或2所述的制膜方法，其特征在于，所述第一溅射阶段的时间为5s～10s；所述第二溅射阶段的时间为5s～10s。
  15. 根据权利要求5所述的制膜方法，其特征在于，所述偏压功率的大小为0kW～2kW。
  16. 根据权利要求1所述的制膜方法，其特征在于，在所述循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求的步骤之前，还包括预加热步骤，所述预加热步骤包括：
    向反应腔室通入第一气体，直至工艺气压达到第一设定气压；
    对晶圆进行加热，直至达到设定温度。
  17. 根据权利要求16所述的制膜方法，其特征在于，所述第一设定气压为1Torr～2Torr；所述设定温度为300℃～400℃。
  18. 根据权利要求16所述的制膜方法，其特征在于，在所述循环进行第一溅射阶段和第二溅射阶段，直至薄膜的厚度满足设定要求的步骤之前，且在所述预加热步骤之后，还包括控压步骤，所述控压步骤包括：
    对所述反应腔室进行抽气；
    同时向所述反应腔室通入第二气体和第三气体，并通过控制所述第二气体和第三气体的气体流量，来使工艺气压在达到第二设定气压时保持恒定。
  19. 根据权利要求18所述的制膜方法，其特征在于，在所述第一溅射阶段和/或第二溅射阶段中，通过调节所述第二气体和第三气体的气体流量比，来调节工艺气压和薄膜的应力。
  20. 根据权利要求18所述的制膜方法，其特征在于，所述第一气体为氩气；第二气体和第三气体分别为氩气和氮气。
  21. 根据权利要求18所述的制膜方法，其特征在于，所述第二设定气压为10mT～200mT。
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