US20050217694A1 - Control of dissolved gas levels in deionized water - Google Patents

Control of dissolved gas levels in deionized water Download PDF

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Publication number
US20050217694A1
US20050217694A1 US11/137,628 US13762805A US2005217694A1 US 20050217694 A1 US20050217694 A1 US 20050217694A1 US 13762805 A US13762805 A US 13762805A US 2005217694 A1 US2005217694 A1 US 2005217694A1
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Prior art keywords
fluid
level
deionized water
intake pipe
nitrogen gas
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Abandoned
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US11/137,628
Inventor
Nilesh Doke
Mona Eissa
Jeffrey Hanson
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Individual
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Priority to US11/137,628 priority Critical patent/US20050217694A1/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02041Cleaning
    • H01L21/02043Cleaning before device manufacture, i.e. Begin-Of-Line process
    • H01L21/02052Wet cleaning only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/231Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids by bubbling
    • B01F23/23105Arrangement or manipulation of the gas bubbling devices
    • B01F23/2312Diffusers
    • B01F23/23124Diffusers consisting of flexible porous or perforated material, e.g. fabric
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/231Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids by bubbling
    • B01F23/23105Arrangement or manipulation of the gas bubbling devices
    • B01F23/2312Diffusers
    • B01F23/23124Diffusers consisting of flexible porous or perforated material, e.g. fabric
    • B01F23/231244Dissolving, hollow fiber membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30Injector mixers
    • B01F25/31Injector mixers in conduits or tubes through which the main component flows
    • B01F25/314Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
    • B01F25/3142Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
    • B01F25/31421Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction the conduit being porous
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30625With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005Apparatus not specifically provided for elsewhere
    • H01L21/67011Apparatus for manufacture or treatment
    • H01L21/67017Apparatus for fluid treatment
    • H01L21/67028Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like
    • H01L21/6704Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing
    • H01L21/67057Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing with the semiconductor substrates being dipped in baths or vessels
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S134/00Cleaning and liquid contact with solids
    • Y10S134/902Semiconductor wafer

Definitions

  • This invention relates to a method and apparatus for optimizing the level of dissolved gasses in the cleaning process that is used to clean wafers having an exposed copper surface.
  • the drawing shows the apparatus for optimizing the level of dissolved gasses in a cleaning tank.
  • CMP Chemical Mechanical Planarization
  • the success of the CMP clean process using megasonic energy in a high pH solution is dependent on the level of dissolved gasses; namely dissolved nitrogen gas. If the level of dissolved nitrogen gases in the cleaning tank is too low then an unwanted level of defects (i.e. residue and particles) is left on the wafer. Conversely, if the level of dissolved nitrogen gasses in the cleaning tank is too high then an unwanted level of copper corrosion occurs.
  • This invention relates to optimizing the level of dissolved gases in the cleaning process so that a “sweet spot” is found where clean-up residue and copper corrosion is minimized.
  • a cleaning tank 2 used in semiconductor manufacturing such as a CMP cleaning tank, holds cleaning fluid 4 and has a megasonic transducer 3 .
  • the cleaning tank 2 may be found in a clean up hood, for example the Cobra model made by Verteq Corporation or a single wafer tank such as the Mirra/Mesa Integrated system made by Applied Materials.
  • the megasonic transducer 3 operates at 350 W. However, it is within the scope of this invention to operate the transducer at a different power level, up to 500 W.
  • the cleaning fluid 4 is a solution created by the mixing of fluids from fluid intake pipes 5 and 6 .
  • Fluid intake pipe 5 contains a high pH solution 7 such as ESC774 from ESC Corporation; however, it is within the scope of this invention to use any high pH fluid (i.e. a fluid having a pH greater than 10).
  • the high pH solution 7 removes slurry particles and carbon based residue from the wafers during the post-CMP clean process.
  • Fluid intake pipe 6 contains deionized water 8 .
  • the level of dissolved nitrogen gas in the deionized water 8 and thereby the level of dissolved nitrogen gas in the cleaning fluid 4 —is affected by a membrane contactor 9 .
  • the use of any membrane contactor is within the scope of this invention, but in the best mode application the membrane contactor is made by Liquicel membrane contactor, made by Membrana GmbH.
  • the deionized water enters the membrane contactor 9 from pipe 10 .
  • the deionized water flows on the shell side of the hydrophobic internal membrane 11 .
  • the membrane contactor 9 can be used to change the level of dissolved gases in the fluid 8 passing through the membrane contactor 9 because the internal membrane 11 is porous to gasses but not to water. In the best mode application the membrane contactor is used to control the level of dissolved nitrogen gas in the deionized water 8 in pipe 6 .
  • the level of dissolved nitrogen gas is increased by adding nitrogen through intake 12 .
  • the nitrogen gas passes through the porous internal membrane 11 and into the flowing deionized water 8 .
  • the level of dissolved nitrogen is decreased by applying a vacuum to intake 13 .
  • the vacuum pulls nitrogen from the deionized water through the porous membrane 11 .
  • the deionized water 8 continues through pipe 6 and into the cleaning tank 2 where it mixes with the high pH fluid 7 from pipe 5 .
  • semiconductor wafers 14 sit in a tray (or “boat) 15 that is suspended in the cleaning fluid 4 by a robot arm 16 .
  • a tray or “boat” 15 that is suspended in the cleaning fluid 4 by a robot arm 16 .
  • increasing the level of dissolved nitrogen gas causes more cavitations resulting from the cleaning fluid 4 interfacing with the copper interconnects on the wafers 14 .
  • the level of dissolved nitrogen gas in the cleaning fluid 4 is too high than an unacceptable level of copper corrosion occurs, thereby decreasing the yield of the wafers 14 .
  • Tests conducted on the best mode application show that the optimum upper limit of dissolved nitrogen gasses in cleaning fluid 4 is 27% saturation; however, levels up to 54% saturation are acceptable. Tests also showed that increasing the level of dissolved nitrogen gas from 54% to 86.5% saturation caused the corrosion defect level to increase from 40 to 15,000 ppm (for a particle size of 0.15 ⁇ m or greater). Furthermore, at the 86.5% saturation level, tests conducted using a KLA SP1 (measurement tool made by KLA Tencor) showed that the amount of haze (which is an indication of copper roughness or corrosion) was eight times greater.
  • the wafers could be cleaned individually.
  • other gases in the deionized water could be controlled using a membrane contactor.
  • the level of dissolved gasses could be controlled on another intake pipe (such as the high pH fluid pipe) or could be controlled by sending the mixture of deionozed water 8 and high pH fluid 7 through the membrane contactor 9 after the fluids are mixed but before they enter the cleaning tank 2 .
  • the functions comprehended by the invention could be accomplished in various stages of the manufacturing process, such as the post probe clean (using, for example, the model FC820 wet hood from DNS Incorporated).
  • this invention can be used with any cleaning tool that uses megasonic energy to clean exposed copper surfaces on wafers.
  • the transducer 3 could be one or more objects of any shape and located anywhere within or around the cleaning tank 2 .

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

An embodiment of the invention is an apparatus having a cleaning tank 2, a megasonic energy source 3, and an intake pipe 6 where a membrane contactor 9 is coupled to the intake pipe 6 to change the concentration of nitrogen gas in the deionized water 8 contained in intake pipe 6 to a range between 5.4% to 54% of saturation. Another embodiment is a method of changing the concentration of nitrogen gas in deionized water 8 to a range between 5.4% to 54% of saturation.

Description

    BACKGROUND OF THE INVENTION
  • This invention relates to a method and apparatus for optimizing the level of dissolved gasses in the cleaning process that is used to clean wafers having an exposed copper surface.
  • BRIEF DESCRIPTION OF THE DRAWINGS
  • The drawing shows the apparatus for optimizing the level of dissolved gasses in a cleaning tank.
  • DETAILED DESCRIPTION OF THE INVENTION
  • Semiconductor manufacturing yield is affected by the quality of the wafer cleaning process. For example, the quality of the Chemical Mechanical Planarization (“CMP”) clean, performed after a copper layer has been polished, affects the yield and reliability of the chips. The success of the CMP clean process using megasonic energy in a high pH solution is dependent on the level of dissolved gasses; namely dissolved nitrogen gas. If the level of dissolved nitrogen gases in the cleaning tank is too low then an unwanted level of defects (i.e. residue and particles) is left on the wafer. Conversely, if the level of dissolved nitrogen gasses in the cleaning tank is too high then an unwanted level of copper corrosion occurs. This invention relates to optimizing the level of dissolved gases in the cleaning process so that a “sweet spot” is found where clean-up residue and copper corrosion is minimized.
  • Several aspects of the invention are described below with reference to example applications for illustration. It should be understood that numerous specific details, relationships, and methods are set forth to provide a full understanding of the invention. One skilled in the relevant art, however, will readily recognize that the invention can be practiced without one or more of the specific details or with other methods. In other instances, well-known structures or operations are not shown in detail to avoid obscuring the invention.
  • Referring to the drawing, a cleaning tank 2 used in semiconductor manufacturing, such as a CMP cleaning tank, holds cleaning fluid 4 and has a megasonic transducer 3. As an example, the cleaning tank 2 may be found in a clean up hood, for example the Cobra model made by Verteq Corporation or a single wafer tank such as the Mirra/Mesa Integrated system made by Applied Materials. In the best mode application the megasonic transducer 3 operates at 350 W. However, it is within the scope of this invention to operate the transducer at a different power level, up to 500 W.
  • The cleaning fluid 4 is a solution created by the mixing of fluids from fluid intake pipes 5 and 6. Fluid intake pipe 5 contains a high pH solution 7 such as ESC774 from ESC Corporation; however, it is within the scope of this invention to use any high pH fluid (i.e. a fluid having a pH greater than 10). The high pH solution 7 removes slurry particles and carbon based residue from the wafers during the post-CMP clean process.
  • Fluid intake pipe 6 contains deionized water 8. In the best mode example, the level of dissolved nitrogen gas in the deionized water 8—and thereby the level of dissolved nitrogen gas in the cleaning fluid 4—is affected by a membrane contactor 9. The use of any membrane contactor is within the scope of this invention, but in the best mode application the membrane contactor is made by Liquicel membrane contactor, made by Membrana GmbH.
  • The deionized water enters the membrane contactor 9 from pipe 10. Upon entering the membrane contactor 9, the deionized water flows on the shell side of the hydrophobic internal membrane 11. The membrane contactor 9 can be used to change the level of dissolved gases in the fluid 8 passing through the membrane contactor 9 because the internal membrane 11 is porous to gasses but not to water. In the best mode application the membrane contactor is used to control the level of dissolved nitrogen gas in the deionized water 8 in pipe 6.
  • During CMP clean, the level of dissolved nitrogen gas is increased by adding nitrogen through intake 12. The nitrogen gas passes through the porous internal membrane 11 and into the flowing deionized water 8. Conversely, the level of dissolved nitrogen is decreased by applying a vacuum to intake 13. The vacuum pulls nitrogen from the deionized water through the porous membrane 11. After passing through the membrane contactor 9, the deionized water 8 continues through pipe 6 and into the cleaning tank 2 where it mixes with the high pH fluid 7 from pipe 5.
  • In the best mode application, semiconductor wafers 14 sit in a tray (or “boat) 15 that is suspended in the cleaning fluid 4 by a robot arm 16. For a stated megasonic power level on the transducer 3, increasing the level of dissolved nitrogen gas causes more cavitations resulting from the cleaning fluid 4 interfacing with the copper interconnects on the wafers 14. However, if the level of dissolved nitrogen gas in the cleaning fluid 4 is too high than an unacceptable level of copper corrosion occurs, thereby decreasing the yield of the wafers 14. Conversely, for a stated megasonic power level on transducer 3, if the level of dissolved nitrogen in the cleaning fluid 4 is too low then a residue of slurry, carbon based residue, particles and/or pad fragments from the CMP process remains on the wafers 14—also decreasing the yield. Therefore, there is an optimum level of dissolved gases for cleaning fluid 4 where the levels of residue defects and corrosion are minimized.
  • Tests conducted on the best mode application show that the optimum upper limit of dissolved nitrogen gasses in cleaning fluid 4 is 27% saturation; however, levels up to 54% saturation are acceptable. Tests also showed that increasing the level of dissolved nitrogen gas from 54% to 86.5% saturation caused the corrosion defect level to increase from 40 to 15,000 ppm (for a particle size of 0.15 μm or greater). Furthermore, at the 86.5% saturation level, tests conducted using a KLA SP1 (measurement tool made by KLA Tencor) showed that the amount of haze (which is an indication of copper roughness or corrosion) was eight times greater.
  • However, there is also a minimum effective level of dissolved nitrogen gas. The defects from the CMP process will not be removed from the wafers 14 unless there is a minimum level of dissolved nitrogen gasses of approximately 5.4% of saturation. A level of dissolved nitrogen gasses above 10.8% of saturation is optimal.
  • Various modifications to the invention as described above are within the scope of the claimed invention. As an example, instead of cleaning a boat of wafers, the wafers could be cleaned individually. Also, instead of controlling the level of dissolved nitrogen gas in the deionized water using the membrane contactor, other gases in the deionized water could be controlled using a membrane contactor. Furthermore, the level of dissolved gasses could be controlled on another intake pipe (such as the high pH fluid pipe) or could be controlled by sending the mixture of deionozed water 8 and high pH fluid 7 through the membrane contactor 9 after the fluids are mixed but before they enter the cleaning tank 2.
  • It is within the scope of the invention to monitor the level of dissolved gasses at any point in the cleaning process (i.e. by evaluating a sample stream using an analyzer made by Orbisphere to monitor the deionized water 8 exiting the membrane contactor). In addition, the functions comprehended by the invention could be accomplished in various stages of the manufacturing process, such as the post probe clean (using, for example, the model FC820 wet hood from DNS Incorporated). Specifically, this invention can be used with any cleaning tool that uses megasonic energy to clean exposed copper surfaces on wafers. For example, the megasonic station on the Ontrak & Lam Synergy cleaners, the megasonic tank on the Mesa, or any Goldfinger megasonic station. Lastly, the transducer 3 could be one or more objects of any shape and located anywhere within or around the cleaning tank 2.
  • While various embodiments of the present invention have been described above, it should be understood that they have been presented by way of example only, and not limitation. Numerous changes to the disclosed embodiments can be made in accordance with the disclosure herein without departing from the spirit or scope of the invention. Thus, the breadth and scope of the present invention should not be limited by any of the above described embodiments. Rather, the scope of the invention should be defined in accordance with the following claims and their equivalents.

Claims (7)

1. An apparatus comprising:
a cleaning station, said cleaning station having a first and second fluid intake pipe;
a megasonic energy source coupled to the inside of said cleaning station; and
a membrane contactor coupled to said first fluid intake pipe, said membrane contactor controlling a partial saturation level of nitrogen gas in a fluid in said first fluid intake pipe, said partial saturation level is in the range between 5.4% to 54% saturation.
2. The apparatus of claim 1 wherein said partial saturation level is 27%.
3. The apparatus of claim 1 wherein said fluid in said first fluid intake pipe is deionized water.
4. The apparatus of claim 1 wherein said second fluid intake pipe contains a high pH fluid.
5. The apparatus of claim 1 wherein said membrane contactor has a first input for providing said nitrogen gas to said fluid through a membrane and a second input for providing a vacuum to said fluid through said membrane.
6. The apparatus of claim 1 wherein at least one semiconductor wafer containing copper features is located inside said cleaning station.
7-15. (canceled)
US11/137,628 2002-12-13 2005-05-25 Control of dissolved gas levels in deionized water Abandoned US20050217694A1 (en)

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US11/137,628 US20050217694A1 (en) 2002-12-13 2005-05-25 Control of dissolved gas levels in deionized water

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US7156111B2 (en) * 2001-07-16 2007-01-02 Akrion Technologies, Inc Megasonic cleaning using supersaturated cleaning solution
US20060201532A1 (en) * 2005-03-14 2006-09-14 Applied Materials, Inc. Semiconductor substrate cleaning system
TWI385226B (en) 2005-09-08 2013-02-11 羅門哈斯電子材料Cmp控股公司 Polymeric barrier removal polishing slurry
US7538969B2 (en) * 2006-08-23 2009-05-26 Imation Corp. Servo pattern with encoded data
CA2934000A1 (en) * 2013-12-20 2015-06-25 Gaia Usa, Inc. Apparatus and method for liquids and gases
WO2018191431A1 (en) 2017-04-12 2018-10-18 Gaia Usa, Inc. Apparatus and method for generating and mixing ultrafine gas bubbles into a high gas concentration aqueous solution
WO2019232273A1 (en) 2018-06-01 2019-12-05 Gaia Usa, Inc. Apparatus in the form of a unitary, single-piece structure configured to generate and mix ultra-fine gas bubbles into a high gas concentration aqueous solution
CN111405914A (en) 2018-06-26 2020-07-10 罗伯特·E·道格拉斯 Intracardiac pump

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US5800626A (en) * 1997-02-18 1998-09-01 International Business Machines Corporation Control of gas content in process liquids for improved megasonic cleaning of semiconductor wafers and microelectronics substrates
US20030015216A1 (en) * 2001-07-16 2003-01-23 Tom Nicolosi Megasonic cleaner probe system with gasified fluid

Patent Citations (3)

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US5800626A (en) * 1997-02-18 1998-09-01 International Business Machines Corporation Control of gas content in process liquids for improved megasonic cleaning of semiconductor wafers and microelectronics substrates
US20030015216A1 (en) * 2001-07-16 2003-01-23 Tom Nicolosi Megasonic cleaner probe system with gasified fluid
US6684890B2 (en) * 2001-07-16 2004-02-03 Verteq, Inc. Megasonic cleaner probe system with gasified fluid

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US20040112404A1 (en) 2004-06-17
US6997192B2 (en) 2006-02-14

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