WO2023045835A1 - Procédé de préparation d'un film de composé métallique - Google Patents

Procédé de préparation d'un film de composé métallique Download PDF

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WO2023045835A1
WO2023045835A1 PCT/CN2022/119220 CN2022119220W WO2023045835A1 WO 2023045835 A1 WO2023045835 A1 WO 2023045835A1 CN 2022119220 W CN2022119220 W CN 2022119220W WO 2023045835 A1 WO2023045835 A1 WO 2023045835A1
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equal
less
wafer
inert gas
reaction chamber
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PCT/CN2022/119220
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Chinese (zh)
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马迎功
郭冰亮
武树波
赵晨光
周麟
宋玲彦
杨健
甄梓杨
翟洪涛
段俊雄
师帅涛
许文学
张璐
崔亚欣
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北京北方华创微电子装备有限公司
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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
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • 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
    • C23C14/3435—Applying energy to the substrate during sputtering
    • C23C14/345—Applying energy to the substrate during sputtering using substrate bias
    • 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
    • C23C14/54—Controlling or regulating the coating process
    • 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
    • C23C14/58—After-treatment
    • C23C14/5826—Treatment with charged particles
    • C23C14/5833—Ion beam bombardment
    • 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
    • C23C14/58—After-treatment
    • C23C14/5873—Removal of material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention relates to the field of semiconductor technology, and more specifically, to a method for preparing a metal compound thin film.
  • PVD Physical vapor deposition
  • a thin film deposition technology is mainly used in the deposition of various functional thin films, and is widely used in semiconductor fields such as integrated circuits, solar cells, and LEDs.
  • AlN thin films have been widely used as buffer layers or piezoelectric layers in LEDs, micro-electro-mechanical systems (Micro-Electro-Mechanical System, MEMS), high electron mobility transistors (High Electron Mobility Transistor, HEMT) and other fields .
  • MEMS Micro-Electro-Mechanical System
  • HEMT High Electron Mobility Transistor
  • the stress of the AlN film is zero. If the stress of the AlN film is too large, the film will be bent or even fall off due to force, which will affect the reliability of the device.
  • AlN films are mainly deposited on Si substrates or SiO 2 substrates, which require stress in the range of 0 ⁇ 100Mpa in MEMS applications. When process parameters such as temperature, sputtering gas, and pressure are optimized, and other process parameters are kept constant, the stress of the AlN film is basically unchanged, and it is difficult to adjust the stress of AlN (with a thickness of 500nm to 1500nm).
  • the purpose of the present invention is to propose a kind of preparation method of metal compound thin film, solve the problem that thin film is bent under force, even falls off, and then improves the reliability of device, described preparation method comprises:
  • Step 1 Put the tray carrying the wafer to be deposited into the reaction chamber and place it above the base;
  • Step 2 Introduce a first mixed gas of a first inert gas and a process gas into the reaction chamber, apply excitation power to the metal target in the reaction chamber, and make the first mixed gas form a plasma, The plasma bombards the metal target to form a metal compound film on the wafer; at the same time, RF bias power is applied to the susceptor to adjust the stress of the metal compound film.
  • step 2 after the step 2, it also includes:
  • Step 3 Introduce a second inert gas into the reaction chamber, and apply radio frequency bias power to the susceptor, so that the second inert gas forms a plasma, and the plasma formed by the second inert gas is The surface of the metal compound film is etched to further adjust the stress of the metal compound film.
  • step 1 after the step 1, and before the step 2, it also includes:
  • Step 101 heating the tray and the wafer to a preset temperature to remove moisture from the tray and the wafer and organic impurities attached to the surface of the wafer.
  • step 101 after the step 101, and before the step 2, it also includes:
  • Step 102 Flowing a third inert gas into the reaction chamber, and applying radio frequency bias power to the susceptor, so that the third inert gas forms a plasma, and the plasma formed by the third inert gas bombarding the surface of the wafer to remove impurities on the surface of the wafer.
  • the method further includes:
  • Step 103 Move the baffle to cover the wafer, pass the second mixed gas of the fourth inert gas and the process gas into the reaction chamber, apply excitation power to the metal target, and make the The second mixed gas forms plasma and performs a pre-sputtering process; after the gas flow rate of the second mixed gas and the excitation power introduced into the reaction chamber are stabilized, the baffle is removed from the crystal The upper part of the circle is removed, and the excitation power and the gas flow rate of the second mixed gas are kept constant.
  • the flow rate of the first inert gas is less than or equal to 200 sccm, and the flow rate of the process gas is less than or equal to 500 sccm; the flow ratio of the process gas to the first inert gas is greater than or equal to 4 and less than or equal to 10,
  • the excitation power applied to the metal target is less than or equal to 10000W, and the radio frequency bias power applied to the base is less than or equal to 1000W.
  • the flow rate of the third inert gas is less than or equal to 200 sccm; the RF bias power applied to the susceptor is greater than or equal to 40W and less than or equal to 100W; the reaction chamber The pressure is greater than or equal to 6mTorr, and less than or equal to 15mTorr.
  • the flow rate of the fourth inert gas is less than or equal to 200 sccm, the flow rate of the process gas is less than or equal to 500 sccm; the flow ratio of the process gas to the fourth inert gas is greater than or equal to 4, and less than or equal to 10, the excitation power applied to the metal target is less than or equal to 10000W.
  • the flow rate of the second inert gas is less than or equal to 200 sccm, and the RF bias power applied to the susceptor is greater than or equal to 150W and less than or equal to 400W.
  • the vacuum degree of the reaction chamber is less than or equal to 5 ⁇ 10 -6 Torr; the temperature of the susceptor is greater than or equal to 400°C and less than or equal to 600°C.
  • the metal target includes aluminum, titanium, hafnium or tantalum, or a compound of aluminum, titanium, hafnium or tantalum.
  • step 2 the plasma formed by the first mixed gas is used to bombard the metal target, and at the same time, the radio frequency bias power is applied to the base, and the radio frequency bias power will be generated on the base
  • a negative bias voltage is formed on the surface, which can optimize the direction of movement of ions in the plasma, so as to adjust the stress of the metal compound film when the metal compound film is formed on the wafer, so that the stress changes from tensile stress to compressive stress, and promotes the film to (002) generates a concentration of crystal orientations, which solves the problem of bending or even falling off of the film under force, thereby improving the reliability of the device.
  • a second inert gas is introduced into the reaction chamber, and a radio frequency bias power is applied to the susceptor.
  • the plasma generated by the second inert gas can engrave the surface of the metal compound thin film. Corrosion can further change the stress from tensile stress to compressive stress, so as to further adjust the stress of the metal compound film.
  • Fig. 1 shows the structural diagram of the magnetron sputtering equipment that the embodiment of the present invention adopts
  • Fig. 2 shows the flowchart of the preparation method of the metal compound film provided by the first embodiment of the present invention
  • Fig. 3 shows the flowchart of the preparation method of the metal compound thin film provided by the second embodiment of the present invention
  • Fig. 4 shows the flowchart of the preparation method of the metal compound film provided by the third embodiment of the present invention.
  • Fig. 5 shows the stress contrast figure of the metal compound film prepared according to two different embodiments of the present invention
  • FIG. 6 shows a comparison chart of thin film XRD test results of metal compound thin films prepared according to the embodiment of the present invention and the prior art.
  • connection should be understood in a broad sense, for example, it can be a fixed connection or a detachable connection. Connected, or integrally connected; it may be mechanically connected, may be directly connected, or may be indirectly connected through an intermediary. Those of ordinary skill in the art can understand the specific meanings of the above terms in the present invention in specific situations.
  • Fig. 1 shows a structural diagram of a magnetron sputtering device used in an embodiment of the present invention.
  • this magnetron sputtering equipment comprises reaction chamber 14, and the top of this reaction chamber 14 is provided with target material 2, and above target material 2 is provided with vacuum cavity 15, and in this vacuum cavity 15 Filled with deionized water, used to cool the target 2, to prevent the target 2 from heating up due to heat release during the sputtering process.
  • a rotatable magnetron 1 is arranged in the vacuum cavity 15, and the magnetron 1 includes inner and outer magnetic poles with opposite polarities, which are used to improve the ionization rate of the gas in the sputtering process, thereby increasing the sputtering rate.
  • a base 9 is provided, and a support 13 is provided on the base 9 for supporting the tray 8 carrying the wafer, so that the tray 8 is located above the base 9 ;
  • a heating tube (not shown) is also provided on the base 9 for radiating heat toward the tray 8 and the wafer above it, so that the wafer can be heated to a preset temperature.
  • a cooling device is also provided in the base 9 for cooling the wafer.
  • the base 9 is liftable, and it can rise from the film transfer position shown in Figure 1 to the process position. During this process, the base 9 will lift the pressure ring 5, so that the base 9, the upper inner Liner 3 and lower inner liner 4 form a closed sputtering environment.
  • a library 10 is also provided on one side of the reaction chamber 14 for accommodating the baffle 7 , and the baffle 7 is used to move out of the library 10 during the pre-sputtering process and move to shield the wafer above.
  • a vacuum pump system 12 is provided at the bottom of the reaction chamber 14 for evacuating the reaction chamber 14 so that the reaction chamber 14 can reach a higher degree of vacuum to meet the vacuum conditions required by the process.
  • the above-mentioned target material 2 is a metal target material, and the metal target material may be a pure metal or a metal compound.
  • the target 2 is electrically connected to the excitation power supply, and the excitation power is used to load the excitation to the target 2, so that the target 2 forms a negative bias voltage relative to the grounded cavity (including the upper lining 3 and the lower lining 4), so that the sputtering
  • the plasma is generated by discharging the jet gas (including N 2 , Ar, O 2 , etc.), the positively charged ions in the plasma are attracted to the target 2, and bombard the surface of the target 2, the sputtered metal atoms are mixed with the plasma Atoms (such as nitrogen atoms) react to form a metal compound and deposit on the surface of the wafer to form a metal compound film.
  • the above excitation power supply is, for example, a DC power supply for loading DC power, a pulsed DC power supply for loading pulsed DC power, or a combination of a DC power supply (or a pulsed DC power supply) and a radio frequency power supply.
  • the first embodiment of the present invention provides a method for preparing a metal compound film, please refer to Figure 2, the method for preparing the metal compound film includes:
  • Step 1 Put the tray carrying the wafer to be deposited into the reaction chamber and place it above the base;
  • Step 2 Introduce the first mixed gas of the first inert gas and the process gas into the reaction chamber, apply excitation power to the metal target in the reaction chamber, make the first mixed gas form plasma, and the plasma bombards the metal target material to form a metal compound film on the wafer; at the same time, RF bias power is applied to the base to adjust the stress of the metal compound film.
  • the above-mentioned first inert gas includes, for example, argon, krypton, etc.; the process gas includes, for example, oxygen, nitrogen, and the like.
  • the first inert gas and the process gas can be connected to the reaction chamber through flow meters.
  • the first inert gas and the process gas are ionized and discharged to generate positively charged plasma, and the positively charged plasma Attracted by and bombards the metal target.
  • the energy of the plasma is high enough, the atoms on the surface of the metal target will escape and be deposited on the wafer, so as to achieve thin film deposition on the wafer surface.
  • the metal atoms escaping from the surface of the target combine with the atoms in the process gas to form metal compounds, they are deposited on the wafer surface and migrate on the wafer surface.
  • the RF bias power applied to the susceptor can promote the metal compounds on the wafer.
  • the surface migrates to a certain direction, and the negative bias voltage formed on the surface of the base by the RF bias power can optimize the movement direction of the ions in the plasma, so as to adjust the stress of the metal compound film when the metal compound film is formed on the wafer, so that the stress
  • the transition from tensile stress to compressive stress promotes the concentration of the film to the (002) crystal orientation, which solves the problem of bending or even falling off of the film under force, thereby improving the reliability of the device.
  • the preparation method of the metal compound thin film provided by the second embodiment of the present invention is an improvement made on the basis of the first embodiment above, specifically, the preparation method of the metal compound thin film also includes steps 1 and Step 2, the two are the same as the above-mentioned first embodiment, and will not be described again here.
  • the preparation method also includes:
  • Step 3 Introduce a second inert gas into the reaction chamber, and apply radio frequency bias power to the susceptor, so that the second inert gas forms a plasma, and the plasma formed by the second inert gas conducts the surface of the metal compound film Etching to further adjust the stress of the metal compound film.
  • the plasma generated by the second inert gas can etch the surface of the metal compound film to etch and remove the lower mass on the film surface.
  • the stress can be further transformed from tensile stress to compressive stress to further adjust the stress of the metal compound film.
  • the above step 3 specifically includes: stop loading the excitation power and radio frequency bias power, and stop the introduction of inert gas and process gas, maintain the heating temperature and The position of the susceptor (process position) remains unchanged; a second inert gas (such as Ar) is introduced into the reaction chamber, and the flow rate of the second inert gas is less than or equal to 200 sccm, preferably greater than or equal to 100 sccm, and less than or equal to 200 sccm.
  • the cold pump gate valve in the vacuum pump system is fully open to ensure that the impurity gas in the reaction chamber can be discharged.
  • Applying radio frequency bias power to the base optionally, the radio frequency bias power applied to the base is greater than or equal to 150W and less than or equal to 400W.
  • the method for preparing a metal compound thin film provided in the second embodiment of the present invention is an improvement made on the basis of the second embodiment above, specifically, the method for preparing a metal compound thin film also includes steps 1, Step 2 and Step 3 are the same as the above-mentioned second embodiment, and will not be described again here.
  • the preparation method further includes at least one of step 101, step 102 and step 103.
  • the preparation method will be described in detail below by taking the deposition of an aluminum nitride film on the surface of the wafer, and the preparation method including step 1, step 2 and step 3, and step 101, step 102 and step 103 as an example.
  • the tray of the wafer such as silicon or silicon dioxide
  • the base that is, the top of the pillar placed on the base
  • adjust the temperature of the base to the temperature required by the process, for example, when depositing aluminum nitride film, the vacuum degree of the reaction chamber is less than 5 ⁇ 10-6Torr
  • the base The temperature is greater than or equal to 400°C and less than or equal to 600°C, such as 500°C.
  • the excitation power loaded to the target can be pulsed DC power, which can avoid the formation of metal nitrides on the surface of the metal target due to the loading of DC power, Escape of metal atoms affecting the metal target.
  • step 1 and before step 2 it also includes:
  • Step 101 heating the tray and the wafer to a preset temperature to remove moisture from the tray and the wafer and organic impurities attached to the surface of the wafer.
  • the tray and the wafer can be heated by the heating tube on the base to slowly raise the temperature to a preset temperature
  • the preset temperature is, for example, greater than or equal to 300° C. and less than or equal to 1000° C., preferably greater than or equal to 450° C. °C, and less than or equal to 800 °C, and maintained for 10s to 200s, preferably 20s to 60s.
  • step 101 and before step 2 it also includes:
  • Step 102 injecting a third inert gas into the reaction chamber, and applying radio frequency bias power to the susceptor, so that the third inert gas forms plasma, and the plasma formed by the third inert gas bombards the surface of the wafer, To remove impurities on the wafer surface.
  • the reaction chamber may be as follows: maintain the heating temperature adopted in step 101, and feed a third inert gas, such as argon (Ar), into the reaction chamber.
  • a third inert gas such as argon (Ar)
  • the flow rate of the third inert gas is less than or equal to 200 sccm, preferably greater than or equal to 100sccm, and less than or equal to 200sccm.
  • the chamber pressure is maintained in a relatively high pressure range, for example greater than or equal to 6 mTorr and less than or equal to 15 mTorr.
  • the radio frequency bias power adopts a lower power range, so that ions in the plasma formed by the third inert gas can bombard the wafer surface to remove impurities and oxidation on the wafer surface substances, reduce wafer surface defects, and increase wafer surface activity.
  • the RF bias power applied to the base is greater than or equal to 40W and less than or equal to 100W.
  • the process pressure that is, the chamber pressure
  • the process pressure can be reduced to about half of the original (such as greater than or equal to 3mTorr, and less than or equal to 8mTorr), and the formal process can be started.
  • Pre-cleaning treatment process ie, step 102).
  • step 103 is also included before step 2:
  • the baffle to the top of the covering wafer, pass the second mixed gas of the fourth inert gas and the process gas into the reaction chamber, apply excitation power to the metal target, make the second mixed gas form plasma, and perform a preliminary Sputtering process; after the gas flow and excitation power of the second mixed gas fed into the reaction chamber are stabilized (the stable index is that the fluctuation range of the gas flow is not greater than ⁇ 0.1%; the fluctuation range of the excitation power is not greater than ⁇ 0.1% %), remove the baffle from above the wafer, and keep the excitation power and the gas flow rate of the second mixed gas constant.
  • the above step 103 is a pre-sputtering process. Specifically, stop feeding the third inert gas, turn off the RF bias power applied to the base, adjust the base to the pre-sputtering station, move the baffle into the reaction chamber, and move it to cover the wafer ; Introducing a second mixed gas of a fourth inert gas (such as Ar) and a process gas (such as N 2 ) into the reaction chamber, wherein the flow rate of the fourth inert gas is less than or equal to 200 sccm, preferably greater than or equal to 15 sccm, and less than or equal to 45 sccm , the flow rate of the process gas is less than or equal to 500 sccm, preferably greater than or equal to 90 sccm, and less than or equal to 300 sccm, the flow ratio of the process gas to the fourth inert gas is greater than or equal to 4, and less than or equal to 10, and the excitation power applied to the metal target is less than or equal to 10
  • the reactive sputtering environment in the reaction chamber is stable, keep the excitation power and gas flow constant, keep the cold pump valve in the vacuum pump system fully open, remove the baffle from the wafer, and keep it for about 1s. Due to the unstable power and gas flow in the initial stage of sputtering in the reaction chamber, the quality of the formed metal compound film is poor. With the help of the above step 103, the metal compound film formed on the wafer can also meet higher quality requirements in the initial stage.
  • the above step 2 is started. Specifically, the excitation power is maintained, the temperature and the process atmosphere are kept constant, and the susceptor is raised to the process position.
  • the distance between the wafer and the target is, for example, greater than or equal to 30 mm and less than or equal to 80 mm, preferably greater than or equal to 40 mm and less than or equal to 60 mm. In this way, both the high growth rate of the film and the crystallization quality of the metal compound film can be guaranteed.
  • a radio frequency bias power of less than or equal to 1000W to the base preferably greater than or equal to 50W, and less than or equal to 300W
  • the higher the applied radio frequency bias power the greater the tendency of the stress of the film to change from tensile stress to compressive stress.
  • the crystallization quality of the metal compound film changes positively with the process temperature.
  • the higher the process temperature the greater the tensile stress of the metal compound film, which requires higher RF bias power to adjust the stress to transform it to compressive stress.
  • the metal atoms such as Al atoms
  • the atoms such as N atoms
  • the voltage power can promote the metal compound to migrate in a certain direction on the wafer surface, and the RF bias power makes the negative bias formed on the surface of the susceptor promote the concentration of the metal compound to the (002) growth crystal direction, thereby adjusting the stress of the metal compound film from tension to Stress changes to compressive stress.
  • the crystallization quality of the metal compound film is better in the crystal direction (002).
  • (002) is the arrangement orientation of the internal atomic structure of the material in solid state physics.
  • the deposition rate is controlled at 10-20 A/s until the thickness of the metal compound film reaches the thickness required by the process.
  • the thickness of the metal compound thin film is generally controlled in the range of 200nm to 1300nm.
  • step 3 After completing the above step 3, stop applying RF bias power to the susceptor, stop gas flow, lower the process temperature, and pump the chamber to a high vacuum.
  • the base is lowered from the process position to the transfer position, and the deposited wafer is moved out of the process chamber to complete the preparation of the metal compound film.
  • step 2 the metal target is bombarded with the plasma formed by the first mixed gas, and at the same time, the RF bias power is applied to the susceptor, and the RF bias power will be A negative bias voltage is formed on the base, which can optimize the direction of movement of ions in the plasma to adjust the stress of the metal compound film when the metal compound film is formed on the wafer, so that the stress changes from tensile stress to compressive stress, promoting The film is concentrated toward the (002) generation crystal direction, which solves the problem of bending or even falling off of the film under force, thereby improving the reliability of the device.
  • the plasma generated by the second inert gas can etch the surface of the metal compound thin film, and the stress can be further relieved from tension.
  • the stress is converted to compressive stress to further adjust the stress of the metal compound film.
  • Fig. 5 shows a stress contrast diagram of aluminum nitride films prepared according to two different embodiments of the present invention.
  • the abscissa is the applied radio frequency bias power (RF Bias)
  • the ordinate is the stress (Stress) of the aluminum nitride film, where the positive number is the tensile stress and the negative number is the compressive stress.
  • the solid line in Fig. 5 shows that when adopting the method in the above-mentioned first embodiment to deposit and form the aluminum nitride film, the RF bias power (Bias Process) is applied to the base, and the magnitude of the applied RF bias power has a great influence on the aluminum nitride The influence of film stress; the dotted line in Fig.
  • FIG. 6 shows a comparison chart of XRD test results of aluminum nitride thin films prepared according to the embodiment of the present invention and the prior art.
  • the abscissa of FIG. 6 is the angle Angle ((002) crystal orientation), and the ordinate is the intensity of aluminum nitride.
  • the dotted line in Fig. 6 indicates that when the aluminum nitride thin film is deposited and formed by the preparation method of the aluminum nitride thin film adopted in the prior art, no radio frequency bias power is applied to the base; the solid line in Fig.
  • a radio frequency bias power is applied to the base.
  • the aluminum nitride film grows more towards the (002) crystal direction.
  • the common knowledge of those skilled in the art when forming an aluminum nitride film, the While growing in the direction of the (002) crystal direction, some parts also grow in the direction of the (102) crystal direction. In order to improve the quality of the film, it is expected that the aluminum nitride film grows in the direction of the (002) crystal direction.

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Abstract

L'invention concerne un procédé de préparation d'un film de composé métallique, comprenant : étape 1 : placer dans une chambre de réaction un plateau portant une tranche sur laquelle un film doit être déposé, le plateau étant situé au-dessus d'une base ; et étape 2 : introduire un premier gaz mélangé d'un premier gaz inerte et d'un gaz de traitement dans la chambre de réaction, et appliquer une puissance d'excitation à une cible métallique dans la chambre de réaction, de sorte que le premier gaz mélangé forme un plasma, et le plasma bombarde la cible métallique pour former un film de composé métallique sur la tranche ; et en même temps, appliquer une puissance de polarisation à fréquence radio à la base pour ajuster la contrainte du film de composé métallique. Dans l'étape 2 de la présente invention, la puissance de polarisation de radiofréquence est appliquée à la base pour ajuster la contrainte du film de composé métallique lorsque le film de composé métallique est formé sur la tranche. Le problème selon lequel un film se déforme et même se détache sous la contrainte est résolu, ce qui améliore la fiabilité d'un dispositif.
PCT/CN2022/119220 2021-09-24 2022-09-16 Procédé de préparation d'un film de composé métallique WO2023045835A1 (fr)

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CN114908326A (zh) * 2022-05-06 2022-08-16 北京北方华创微电子装备有限公司 半导体工艺设备及形成叠层薄膜结构的方法

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