WO2010101759A2 - Non destructive selective deposition removal of non-metallic deposits from aluminum containing substrates - Google Patents

Non destructive selective deposition removal of non-metallic deposits from aluminum containing substrates Download PDF

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Publication number
WO2010101759A2
WO2010101759A2 PCT/US2010/025353 US2010025353W WO2010101759A2 WO 2010101759 A2 WO2010101759 A2 WO 2010101759A2 US 2010025353 W US2010025353 W US 2010025353W WO 2010101759 A2 WO2010101759 A2 WO 2010101759A2
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Prior art keywords
solution
faceplate
sdr
deposit
substrate
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PCT/US2010/025353
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French (fr)
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WO2010101759A3 (en
Inventor
Liyuan Bao
Anbei Jiang
Sio On Lo
Yukari Nishimura
Joseph F. Sommers
Samantha S.H. Tan
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Applied Materials Inc
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Applied Materials Inc
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Priority to EP10749118.5A priority Critical patent/EP2404314A4/en
Priority to KR1020117022945A priority patent/KR101279455B1/en
Priority to CN201080010398.7A priority patent/CN102341892B/en
Publication of WO2010101759A2 publication Critical patent/WO2010101759A2/en
Publication of WO2010101759A3 publication Critical patent/WO2010101759A3/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4407—Cleaning of reactor or reactor parts by using wet or mechanical methods
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/12—Light metals
    • C23G1/125—Light metals aluminium
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/24—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using chemical vapour deposition [CVD]
    • 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
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/582—Recycling of unreacted starting or intermediate materials

Definitions

  • Embodiments of the present invention relate to the field of chamber component cleaning and refurbishment.
  • the fabrication of semiconductor devices typically comprises forming multiple layers, including non-metallic layers such as interlayer dielectrics, etch stop layers, and passivation layers. Many of these layers are often deposited using chemical vapor deposition (CVD) methods. Such deposition methods also form deposits of the deposition species on internal chamber components such as a faceplate, also known as a showerhead, of a gas distribution assembly. [0004] Deposits must be routinely removed from the internal chamber surfaces so that they do not serve as a contamination source. Plasma cleaning chemistries can be utilized to clean the chamber components in situ. Alternatively the chamber components can be removed from the chamber and cleaned in solution ex situ. Such cleaning solutions generally comprise a chemistry of nitric acid (HN O 3 ) and hydrofluoric acid (HF).
  • HN O 3 nitric acid
  • HF hydrofluoric acid
  • the cleaning solution is a selective deposition removal (SDR) solution for selectively removing a non-metallic deposit from an aluminum containing substrate.
  • the SDR solution comprises at least one acid, a pH buffer to donate a hydronium ion, a straight or branched chain-diol or - triol from the C 2 to Ce chain to protect the aluminum containing substrate from the acid, and water (H 2 O).
  • the SDR solution comprises, in wt% of the solution, 15.5% +/- 2% HF or buffered HF acid, 3.8% +/- 0.5% NH 4 F pH buffer, 59.7% +/- 5% ethylene glycol, and the balance H 2 O.
  • the SDR solution may be contacted with the aluminum containing substrate to remove the non-metallic deposit without substantially reacting with the aluminum containing substrate.
  • aluminum containing substrates such as aluminum faceplates can be cleaned without substantially etching the faceplate holes, thereby preserving the hole diameter integrity and increasing the number of times the faceplate may be cleaned or refurbished while remaining within processing hole diameter tolerances.
  • FIG. 1 is a top view illustration of a faceplate including multiple holes.
  • FIG. 2A- FIG. 2D are a series of top view images of a faceplate hole illustrating the removal of BLOk.TM deposits for different SDR cleaning solution exposure times at room temperature.
  • FIG. 3 is a chart illustrating flow measurements through individual faceplate holes for different SDR cleaning solution exposure times at room temperature.
  • FIG. 4 is a chart illustrating individual faceplate hole size measurements for different SDR cleaning solution exposure times at room temperature.
  • FIG. 5A is a top view image of a faceplate illustrating surface staining due to arcing across holes pre-SDR cleaning.
  • FIG. 5B is a top view image of a faceplate illustrating the removal of surface staining due to arcing across holes post-SDR cleaning for 180 minutes at room temperature.
  • Embodiments of the present invention disclose a cleaning solution and method for removing deposits from chamber component surfaces.
  • Various embodiments described herein are described with reference to figures. However, certain embodiments may be practiced without one or more of these specific details, or in combination with other known methods and configurations. In the following description, numerous specific details are set forth, such as compositions, and processes, etc., in order to provide a thorough understanding of the present invention.
  • Reference throughout this specification to "one embodiment” or “an embodiment” means that a particular feature, configuration, composition, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. Thus, the appearances of the phrase “in one embodiment” or “an embodiment” in various places throughout this specification are not necessarily referring to the same embodiment of the invention.
  • the particular features, configurations, compositions, or characteristics may be combined in any suitable manner in one or more embodiments.
  • non-metallic deposits can be selectively removed from aluminum containing substrates such as aluminum faceplates using a selective deposition removal (SDR) solution.
  • SDR selective deposition removal
  • the SDR solution does not substantially etch the faceplate holes, thereby preserving the hole diameter integrity and increasing the number of times the faceplate may be cleaned or refurbished while remaining within processing hole diameter tolerances.
  • the SDR solution comprises, in wt% of the solution, 15.5% +/- 2% HF or buffered HF acid, 3.8% +/- 0.5% NH 4 F pH buffer, 59.7% +/- 5% ethylene glycol, and the balance H 2 O.
  • the deposits that may be removed using the methods described herein include non-metallic materials, non-metallic oxides such as silicon oxide (SiO 2 ), carbon-doped oxides (CDO), silicon-carbon-hydrogen (SiCH), non-metallic nitrides such as silicon nitride (Si 3 N 4 ), non-metallic carbides such as silicon carbide (SiC), and other non-metallic dielectric materials.
  • the deposits may also include residues associated with plasma cleaning of a processing chamber component such as AlF 3 .
  • An example of a processing chamber component that may be cleaned or refurbished using the methods described herein is an aluminum faceplate from the PRODUCER.RTM. chemical vapor deposition (CVD) reactor, available from Applied Materials, Inc. of Santa Clara, Calif. Embodiments may also be utilized to clean or refurbish other aluminum containing substrates such as aluminum and aluminum alloy substrates.
  • selective removing is intended to mean removing or stripping a deposit from a substrate without substantially etching or eroding the underlying substrate.
  • without substantially etching is intended to mean no detectable attack on the underlying substrate as determined by visual inspection or microscopic measurement to the ten thousandths of an inch (0.0001 inch).
  • the cleaning solution is a selective deposition removal (SDR) solution for selectively removing a non-metallic deposit from an aluminum containing substrate.
  • the SDR solution comprises at least one acid, a pH buffer, a straight or branched chain-diol or -triol from the C 2 to Ce chain to protect the aluminum containing substrate from the acid, and water (H 2 O).
  • the SDR solution comprises, in wt% of the solution, 15.5% +/- 2% HF or buffered HF acid, 3.8% +/- 0.5% NH 4 F pH buffer, 59.7% +/- 5% ethylene glycol, and the balance H 2 O.
  • the selective removal of the non-metallic deposit from an aluminum containing substrate is associated with the presence of a straight or branched chain-diol or -triol from the C 2 to Ce chain such as ethylene glycol in an amount sufficient to form an ethoxide layer on at least one portion of the aluminum containing substrate not covered with the deposit, i.e. the exposed substrate. Due to this protective ethoxide layer, the aluminum substrate is protected from being attacked by the acid in the SDR solution such as HF. The protective ethoxide layer may form on a portion of the substrate not originally covered with a deposit, as well as form after the deposit is removed from a portion of the substrate.
  • the ethylene glycol protects the substrate from attack by the acid component in the SDR solution during prolonged exposure times of 180 minutes or longer.
  • the substrate protector component may include any straight or branched chain-diol or -triol from the C 2 to Ce chain such as propylene glycol, butanediol, ethylene glycol, or glycerol and combinations thereof at 59.7% +/- 5% by weight of the SDR solution.
  • the acid component comprises 15.5% +/- 2% by weight of the SDR solution.
  • the acid component comprises a fluorine ion, such as HF or buffered HF.
  • the buffered HF is 49% by wt HF, with the remainder water.
  • the acid may comprise other acids such as hydrochloric, sulfuric, nitric, sodium bifluride, ammonium fluoroborate, and barium fluoride. Any one or a combination of these ingredients may be present in the SDR solution in amount ranging from 15.5% +/- 2% by weight of the SDR solution.
  • the acid component may be 49% by weight buffered HF comprising 15.5 from 15.5% +/- 2% by weight of the SDR solution.
  • the pH buffer component comprises 3.8% +/- 0.5% by weight of the SDR solution.
  • the pH buffer comprises a component which is able to donate a hydronium ion (H + ) so that the pH of the SDR solution does not significantly change during deposit removal, and from substrate to substrate sequentially cleaned in the same SDR solution bath. As the acid component of the SDR solution reacts with the deposit hydronium is consumed.
  • the pH buffer component comprises ammonium fluoride (NH 4 F).
  • the remainder of the SDR solution is comprised of water. Though additives such as surfactants and pH modifiers may be included in the SDR solution in place of or part of the water balance.
  • the SDR solution may be applied to a substrate utilizing several available techniques such as exposing the substrate to a timed immersion in a wet chemical bath or a spray from a chemical spray tool until the deposit is completely removed. Such a process can be multi-step in so far as there may be a cycle of strip-inspect- strip-inspect until removal is complete.
  • an aluminum containing substrate is submerged in a bath of SDR solution to remove the non-metallic deposit without substantially reacting with the aluminum containing substrate. Necessary exposure time to the SDR solution may depend upon the deposit composition and thickness.
  • the deposit is a non-metallic oxide such as silicon oxide (SiO 2 ), carbon-doped oxide (CDO), silicon-carbon-hydrogen (SiCH), non-metallic nitride such as silicon nitride (Si 3 N 4 ), non-metallic carbide such as silicon carbide (SiC), or other non-metallic dielectric material.
  • the deposit is an AlF 3 residue.
  • the deposit may be a BlOk.TM film, which is an amorphous film composed of silicon, carbon and hydrogen (a-SiC:H), having a thickness of several microns.
  • the aluminum containing substrate is a faceplate consisting essentially of aluminum.
  • the faceplate can be from the PRODUCER.RTM. chemical vapor deposition (CVD) reactor.
  • FIG. 1 is a top view illustration of a faceplate 100 including a plurality of holes 102. Throughout various locations in the present disclosure reference is made to a specific hole number in the faceplate 100. For illustrative purposes only, holes 1-24 are located along an outer ring A, holes 25-40 are located along a middle ring B, holes 41-48 are located along an inner ring D, and hole 49 is located in the center C of faceplate 100.
  • FIG. 2A - FIG. 2D are a series of top view images of a faceplate hole 202 illustrating the removal of BLOk.TM (a SiC based material) deposits 204 for different SDR cleaning solution exposure times at room temperature.
  • BLOk.TM deposits are visible prior to cleaning with SDR solution in FIG. 2A
  • the BLOk.TM deposits 204 are partially removed after being submerged in SDR solution at room temperature for 120 minutes in FIG. 2B.
  • the BLOk.TM deposits 204 are completely removed after being submerged in SDR solution at room temperature for 180 minutes in FIG. 2C, and after being submerged in SDR solution at room temperature for 300 minutes in FIG. 2D.
  • FIG. 3 is a chart illustrating flow measurements through individual faceplate holes initially covered with BLOk.TM deposits for different SDR cleaning solution exposure times at room temperature, with the individual faceplate holes corresponding to those illustrated in FIG. 1.
  • the flow readings through the faceplate holes is restricted and non-uniform.
  • the flow rate reading is increased and more uniform.
  • the faceplate in SDR solution for 180 minutes flow readings and uniformity is again increased. Measurements after 300 minutes are similar to those at 180 minutes indicating that the BLOk.TM deposits are completely removed after 180 minutes. Accordingly, the results of FIG. 2 and FIG. 3 are consistent that BLOk.TM deposits are completely removed after being submerged in SDR solution at room temperature for 180 minutes.
  • FIG. 4 is a chart illustrating individual faceplate hole size microscopic measurements for different SDR cleaning solution exposure times at room temperature.
  • the faceplate has a uniform hole size of 0.0161 inches prior to being exposed to SDR solution. Even after being submerged in SDR solution for an interval of 300 minutes the microscopically measured hole size does not increase. Accordingly, the measurements show that there is no substantial change in hole size after immersion in SDR solution at room temperature for 300 minutes. This represents a significant improvement over conventional removal solutions, such as HNO 3 /HF solutions which also attack the aluminum faceplates and result in increased hole sizes after shorter exposure times. As illustrated in FIG.
  • the diameter of the faceplate holes did not increase when microscopically measured to the ten thousandths of an inch (0.0001 inch). Accordingly, utilizing embodiments of the present invention, aluminum containing substrates such as aluminum faceplates can be cleaned without substantially etching the faceplate holes, thereby preserving the hole diameter integrity and increasing the number of times the faceplate may be cleaned or refurbished while remaining within processing hole diameter tolerances.
  • FIG. 5A is a top view image of a faceplate illustrating surface staining (indicated by the comparatively darker holes) due to arcing across holes 510 pre-SDR cleaning.
  • FIG. 5B the surface staining due to arcing across holes 510 is completely removed after cleaning in SDR solution for 180 minutes at room temperature. Where surface staining is present due to arcing across holes, the deposit may be partially or completely burned off at the arcing sites.
  • the SDR solution and cleaning methods in accordance with embodiments also allow for the independent adjustment of the surface texture (or surface roughness) since the SDR solution does not substantially etch aluminum.
  • the post treatment may include exposing the substrate to a 90/10 NHO 3 /HF chemistry for several minutes, the post treatment can be utilized to roughen the surface of the substrate.

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  • General Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
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Abstract

Non-metallic deposits are selectively removed from aluminum containing substrates such as aluminum faceplates using a selective deposition removal (SDR) solution. The SDR solution does not substantially etch the faceplate holes, thereby preserving the hole diameter integrity and increasing the number of times the faceplate may be cleaned or refurbished while remaining within processing hole diameter tolerances. In an embodiment, the SDR solution comprises, in wt% of the solution, 15.5% +/- 2% HF or buffered HF acid, 3.8% +/- 0.5% NH4F pH buffer, 59.7% +/- 5% ethylene glycol, and the balance H2O.

Description

NON DESTRUCTIVE SELECTIVE DEPOSITION REMOVAL OF NON-METALLIC DEPOSITS FROM ALUMINUM CONTAINING
SUBSTRATES
RELATED APPLICATIONS
[0001] The present patent application is related to and hereby claims the priority benefit of U.S. Patent Application No. 12/709,369 filed February 19, 2010, which claims the priority benefit of U.S. Provisional Patent Application No. 61/156,728, filed March 2, 2009.
BACKGROUND FIELD
[0002] Embodiments of the present invention relate to the field of chamber component cleaning and refurbishment.
BACKGROUND INFORMATION
[0003] The fabrication of semiconductor devices typically comprises forming multiple layers, including non-metallic layers such as interlayer dielectrics, etch stop layers, and passivation layers. Many of these layers are often deposited using chemical vapor deposition (CVD) methods. Such deposition methods also form deposits of the deposition species on internal chamber components such as a faceplate, also known as a showerhead, of a gas distribution assembly. [0004] Deposits must be routinely removed from the internal chamber surfaces so that they do not serve as a contamination source. Plasma cleaning chemistries can be utilized to clean the chamber components in situ. Alternatively the chamber components can be removed from the chamber and cleaned in solution ex situ. Such cleaning solutions generally comprise a chemistry of nitric acid (HN O3) and hydrofluoric acid (HF).
SUMMARY
[0005] Embodiments of the present invention disclose a cleaning solution and method for removing deposits from chamber components. [0006] In an embodiment, the cleaning solution is a selective deposition removal (SDR) solution for selectively removing a non-metallic deposit from an aluminum containing substrate. In an embodiment, the SDR solution comprises at least one acid, a pH buffer to donate a hydronium ion, a straight or branched chain-diol or - triol from the C2 to Ce chain to protect the aluminum containing substrate from the acid, and water (H2O). In an embodiment, the SDR solution comprises, in wt% of the solution, 15.5% +/- 2% HF or buffered HF acid, 3.8% +/- 0.5% NH4F pH buffer, 59.7% +/- 5% ethylene glycol, and the balance H2O.
[0007] In an embodiment, the SDR solution may be contacted with the aluminum containing substrate to remove the non-metallic deposit without substantially reacting with the aluminum containing substrate. Utilizing embodiments of the present invention, aluminum containing substrates such as aluminum faceplates can be cleaned without substantially etching the faceplate holes, thereby preserving the hole diameter integrity and increasing the number of times the faceplate may be cleaned or refurbished while remaining within processing hole diameter tolerances.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a top view illustration of a faceplate including multiple holes.
[0009] FIG. 2A- FIG. 2D are a series of top view images of a faceplate hole illustrating the removal of BLOk.TM deposits for different SDR cleaning solution exposure times at room temperature.
[0010] FIG. 3 is a chart illustrating flow measurements through individual faceplate holes for different SDR cleaning solution exposure times at room temperature.
[0011] FIG. 4 is a chart illustrating individual faceplate hole size measurements for different SDR cleaning solution exposure times at room temperature.
[0012] FIG. 5A is a top view image of a faceplate illustrating surface staining due to arcing across holes pre-SDR cleaning.
[0013] FIG. 5B is a top view image of a faceplate illustrating the removal of surface staining due to arcing across holes post-SDR cleaning for 180 minutes at room temperature. DETAILED DESCRIPTION
[0014] Embodiments of the present invention disclose a cleaning solution and method for removing deposits from chamber component surfaces. [0015] Various embodiments described herein are described with reference to figures. However, certain embodiments may be practiced without one or more of these specific details, or in combination with other known methods and configurations. In the following description, numerous specific details are set forth, such as compositions, and processes, etc., in order to provide a thorough understanding of the present invention. Reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, configuration, composition, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. Thus, the appearances of the phrase "in one embodiment" or "an embodiment" in various places throughout this specification are not necessarily referring to the same embodiment of the invention. Furthermore, the particular features, configurations, compositions, or characteristics may be combined in any suitable manner in one or more embodiments.
[0016] In accordance with embodiments, non-metallic deposits can be selectively removed from aluminum containing substrates such as aluminum faceplates using a selective deposition removal (SDR) solution. The SDR solution does not substantially etch the faceplate holes, thereby preserving the hole diameter integrity and increasing the number of times the faceplate may be cleaned or refurbished while remaining within processing hole diameter tolerances. In an embodiment, the SDR solution comprises, in wt% of the solution, 15.5% +/- 2% HF or buffered HF acid, 3.8% +/- 0.5% NH4F pH buffer, 59.7% +/- 5% ethylene glycol, and the balance H2O.
[0017] The deposits that may be removed using the methods described herein include non-metallic materials, non-metallic oxides such as silicon oxide (SiO2), carbon-doped oxides (CDO), silicon-carbon-hydrogen (SiCH), non-metallic nitrides such as silicon nitride (Si3N4), non-metallic carbides such as silicon carbide (SiC), and other non-metallic dielectric materials. The deposits may also include residues associated with plasma cleaning of a processing chamber component such as AlF3. [0018] An example of a processing chamber component that may be cleaned or refurbished using the methods described herein is an aluminum faceplate from the PRODUCER.RTM. chemical vapor deposition (CVD) reactor, available from Applied Materials, Inc. of Santa Clara, Calif. Embodiments may also be utilized to clean or refurbish other aluminum containing substrates such as aluminum and aluminum alloy substrates.
[0019] As used herein, "selectively removing" (or derivations thereof) is intended to mean removing or stripping a deposit from a substrate without substantially etching or eroding the underlying substrate. As used herein "without substantially etching" (or derivations thereof) is intended to mean no detectable attack on the underlying substrate as determined by visual inspection or microscopic measurement to the ten thousandths of an inch (0.0001 inch).
[0020] In an embodiment, the cleaning solution is a selective deposition removal (SDR) solution for selectively removing a non-metallic deposit from an aluminum containing substrate. In an embodiment, the SDR solution comprises at least one acid, a pH buffer, a straight or branched chain-diol or -triol from the C2 to Ce chain to protect the aluminum containing substrate from the acid, and water (H2O). In an embodiment, the SDR solution comprises, in wt% of the solution, 15.5% +/- 2% HF or buffered HF acid, 3.8% +/- 0.5% NH4F pH buffer, 59.7% +/- 5% ethylene glycol, and the balance H2O.
[0021] It is believed that the selective removal of the non-metallic deposit from an aluminum containing substrate is associated with the presence of a straight or branched chain-diol or -triol from the C2 to Ce chain such as ethylene glycol in an amount sufficient to form an ethoxide layer on at least one portion of the aluminum containing substrate not covered with the deposit, i.e. the exposed substrate. Due to this protective ethoxide layer, the aluminum substrate is protected from being attacked by the acid in the SDR solution such as HF. The protective ethoxide layer may form on a portion of the substrate not originally covered with a deposit, as well as form after the deposit is removed from a portion of the substrate. As a result, the ethylene glycol protects the substrate from attack by the acid component in the SDR solution during prolonged exposure times of 180 minutes or longer. In other embodiments, the substrate protector component may include any straight or branched chain-diol or -triol from the C2 to Ce chain such as propylene glycol, butanediol, ethylene glycol, or glycerol and combinations thereof at 59.7% +/- 5% by weight of the SDR solution.
[0022] In an embodiment, the acid component comprises 15.5% +/- 2% by weight of the SDR solution. In an embodiment, the acid component comprises a fluorine ion, such as HF or buffered HF. In an embodiment, the buffered HF is 49% by wt HF, with the remainder water. In another embodiment, the acid may comprise other acids such as hydrochloric, sulfuric, nitric, sodium bifluride, ammonium fluoroborate, and barium fluoride. Any one or a combination of these ingredients may be present in the SDR solution in amount ranging from 15.5% +/- 2% by weight of the SDR solution. For example, the acid component may be 49% by weight buffered HF comprising 15.5 from 15.5% +/- 2% by weight of the SDR solution.
[0023] In an embodiment, the pH buffer component comprises 3.8% +/- 0.5% by weight of the SDR solution. In an embodiment, the pH buffer comprises a component which is able to donate a hydronium ion (H+) so that the pH of the SDR solution does not significantly change during deposit removal, and from substrate to substrate sequentially cleaned in the same SDR solution bath. As the acid component of the SDR solution reacts with the deposit hydronium is consumed. In an embodiment, the pH buffer component comprises ammonium fluoride (NH4F). [0024] The remainder of the SDR solution is comprised of water. Though additives such as surfactants and pH modifiers may be included in the SDR solution in place of or part of the water balance.
[0025] The SDR solution may be applied to a substrate utilizing several available techniques such as exposing the substrate to a timed immersion in a wet chemical bath or a spray from a chemical spray tool until the deposit is completely removed. Such a process can be multi-step in so far as there may be a cycle of strip-inspect- strip-inspect until removal is complete.
[0026] In an embodiment, an aluminum containing substrate is submerged in a bath of SDR solution to remove the non-metallic deposit without substantially reacting with the aluminum containing substrate. Necessary exposure time to the SDR solution may depend upon the deposit composition and thickness. In an embodiment, the deposit is a non-metallic oxide such as silicon oxide (SiO2), carbon-doped oxide (CDO), silicon-carbon-hydrogen (SiCH), non-metallic nitride such as silicon nitride (Si3N4), non-metallic carbide such as silicon carbide (SiC), or other non-metallic dielectric material. In an embodiment, the deposit is an AlF3 residue. In an embodiment, the deposit may be a BlOk.TM film, which is an amorphous film composed of silicon, carbon and hydrogen (a-SiC:H), having a thickness of several microns. In an embodiment the aluminum containing substrate is a faceplate consisting essentially of aluminum. For example, the faceplate can be from the PRODUCER.RTM. chemical vapor deposition (CVD) reactor. [0027] FIG. 1 is a top view illustration of a faceplate 100 including a plurality of holes 102. Throughout various locations in the present disclosure reference is made to a specific hole number in the faceplate 100. For illustrative purposes only, holes 1-24 are located along an outer ring A, holes 25-40 are located along a middle ring B, holes 41-48 are located along an inner ring D, and hole 49 is located in the center C of faceplate 100.
[0028] FIG. 2A - FIG. 2D are a series of top view images of a faceplate hole 202 illustrating the removal of BLOk.TM (a SiC based material) deposits 204 for different SDR cleaning solution exposure times at room temperature. As shown, BLOk.TM deposits are visible prior to cleaning with SDR solution in FIG. 2A, the BLOk.TM deposits 204 are partially removed after being submerged in SDR solution at room temperature for 120 minutes in FIG. 2B. The BLOk.TM deposits 204 are completely removed after being submerged in SDR solution at room temperature for 180 minutes in FIG. 2C, and after being submerged in SDR solution at room temperature for 300 minutes in FIG. 2D.
[0029] FIG. 3 is a chart illustrating flow measurements through individual faceplate holes initially covered with BLOk.TM deposits for different SDR cleaning solution exposure times at room temperature, with the individual faceplate holes corresponding to those illustrated in FIG. 1. As shown, prior to cleaning with SDR solution the flow readings through the faceplate holes is restricted and non-uniform. After submerging the faceplate in SDR solution for 120 minutes at room temperature the flow rate reading is increased and more uniform. After submerging the faceplate in SDR solution for 180 minutes flow readings and uniformity is again increased. Measurements after 300 minutes are similar to those at 180 minutes indicating that the BLOk.TM deposits are completely removed after 180 minutes. Accordingly, the results of FIG. 2 and FIG. 3 are consistent that BLOk.TM deposits are completely removed after being submerged in SDR solution at room temperature for 180 minutes.
[0030] FIG. 4 is a chart illustrating individual faceplate hole size microscopic measurements for different SDR cleaning solution exposure times at room temperature. As shown in FIG. 4, the faceplate has a uniform hole size of 0.0161 inches prior to being exposed to SDR solution. Even after being submerged in SDR solution for an interval of 300 minutes the microscopically measured hole size does not increase. Accordingly, the measurements show that there is no substantial change in hole size after immersion in SDR solution at room temperature for 300 minutes. This represents a significant improvement over conventional removal solutions, such as HNO3/HF solutions which also attack the aluminum faceplates and result in increased hole sizes after shorter exposure times. As illustrated in FIG. 4 the diameter of the faceplate holes did not increase when microscopically measured to the ten thousandths of an inch (0.0001 inch). Accordingly, utilizing embodiments of the present invention, aluminum containing substrates such as aluminum faceplates can be cleaned without substantially etching the faceplate holes, thereby preserving the hole diameter integrity and increasing the number of times the faceplate may be cleaned or refurbished while remaining within processing hole diameter tolerances.
[0031] The SDR solution and cleaning methods in accordance with embodiments provide additional benefits over conventional cleaning methods. For example, the SDR solution can effectively clean faceplates having surface staining arcing holes without substantially etching the arcing holes. FIG. 5A is a top view image of a faceplate illustrating surface staining (indicated by the comparatively darker holes) due to arcing across holes 510 pre-SDR cleaning. As illustrated in FIG. 5B the surface staining due to arcing across holes 510 is completely removed after cleaning in SDR solution for 180 minutes at room temperature. Where surface staining is present due to arcing across holes, the deposit may be partially or completely burned off at the arcing sites. As a result, conventional cleaning solutions preferentially attack the holes of an aluminum faceplate where arcing has occurred which results in an increased hole size. Utilizing embodiments of the present invention, aluminum faceplates including surface staining due to arcing across holes can be cleaned to remove the surface staining without increasing the hole size. [0032] The SDR solution and cleaning methods in accordance with embodiments also allow for the independent adjustment of the surface texture (or surface roughness) since the SDR solution does not substantially etch aluminum. For example, where the substrate is to be used in a CVD chamber it may be preferred to have a specific surface roughness to trap the deposits and prevent the deposits from contaminating the workpiece being processed. In an embodiment, the post treatment may include exposing the substrate to a 90/10 NHO3/HF chemistry for several minutes, the post treatment can be utilized to roughen the surface of the substrate.
[0033] In the foregoing specification, various embodiments of the invention have been described. It will, however, be evident that various modifications and changes may be made thereto without departing from the broader spirit and scope of the invention as set forth in the appended claims. The specification and drawings are, accordingly, to be regarded in an illustrative sense rather than a restrictive sense.

Claims

CLAIMSWhat is claimed is:
1. A method for selectively removing a non-metallic deposit from an aluminum containing substrate comprising: contacting the aluminum containing substrate with a solution until the non- metallic deposit is removed from said substrate, the solution comprising: an acid; a pH buffer to donate a hydronium ion; a straight or branched chain-diol or -triol from the C2 to Ce chain; and water.
2. The method of claim 1, wherein the solution comprises, in weight % of the solution:
15.5% +/- 2% HF or buffered HF acid; 3.8% +/- 0.5% NH4F pH buffer; 59.7% +/- 5% ethylene glycol; and water.
3. The method of claim 2, wherein said deposit is a non-metallic dielectric.
4. The method of claim 2, wherein said deposit is selected from the group consisting of a-SiC:H, SiO2, SiC, and AlF3.
5. The method of claim 2, wherein said deposit is selected from the group consisting of a-SiC:H, SiO2 and SiC.
6. The method of claim 2, wherein said deposit is AlF3.
7. The method of claim 4, wherein contacting comprises submersing the substrate in said solution for 180 minutes or longer.
8. The method of claim 7, wherein said substrate is a faceplate including a plurality of holes having a diameter, and said diameter of said plurality of holes is not increased by 0.0001 inch during said contacting.
9. The method of claim 8, further comprising exposing said faceplate to an acid to increase the surface roughness of a surface of said faceplate after contacting said faceplate with said solution.
10. The method of claim 8, wherein said substrate includes surface staining due to arcing across holes.
11. The method of claim 7, wherein said contacting is performed at approximately room temperature.
PCT/US2010/025353 2009-03-02 2010-02-25 Non destructive selective deposition removal of non-metallic deposits from aluminum containing substrates Ceased WO2010101759A2 (en)

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EP10749118.5A EP2404314A4 (en) 2009-03-02 2010-02-25 SELECTIVE AND NON-DESTRUCTIVE REMOVAL OF NON-METALLIC DEPOSITS OF SUBSTRATES CONTAINING ALUMINUM
KR1020117022945A KR101279455B1 (en) 2009-03-02 2010-02-25 Non destructive selective deposition removal of non-metallic deposits from aluminum containing substrates
CN201080010398.7A CN102341892B (en) 2009-03-02 2010-02-25 Non-destructive and selective deposition removal method for the removal of non-metallic deposits from aluminum-containing substrates

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US12/709,369 US8398779B2 (en) 2009-03-02 2010-02-19 Non destructive selective deposition removal of non-metallic deposits from aluminum containing substrates

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US8398779B2 (en) 2013-03-19
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TWI450772B (en) 2014-09-01
CN102341892B (en) 2014-09-17
KR20110132424A (en) 2011-12-07
EP2404314A4 (en) 2016-08-10
KR101279455B1 (en) 2013-06-26
US20100218788A1 (en) 2010-09-02
WO2010101759A3 (en) 2010-11-18
TW201032911A (en) 2010-09-16

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