WO2009032459A1 - Appareil faisant appel à des fluides électrostatiques distribués par électronébulisation pour nettoyer des surfaces, laissant une contamination résiduelle réduite et procédé correspondant - Google Patents

Appareil faisant appel à des fluides électrostatiques distribués par électronébulisation pour nettoyer des surfaces, laissant une contamination résiduelle réduite et procédé correspondant Download PDF

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Publication number
WO2009032459A1
WO2009032459A1 PCT/US2008/072038 US2008072038W WO2009032459A1 WO 2009032459 A1 WO2009032459 A1 WO 2009032459A1 US 2008072038 W US2008072038 W US 2008072038W WO 2009032459 A1 WO2009032459 A1 WO 2009032459A1
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WO
WIPO (PCT)
Prior art keywords
liquid
electrode
opening
source
solution
Prior art date
Application number
PCT/US2008/072038
Other languages
English (en)
Inventor
John F. Mahoney
James K. Finster
Julius Perel
Original Assignee
Ehd Technology Group, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ehd Technology Group, Inc. filed Critical Ehd Technology Group, Inc.
Publication of WO2009032459A1 publication Critical patent/WO2009032459A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02041—Cleaning
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus 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
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H01L21/67028—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like
    • H01L21/6704—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing
    • H01L21/67051—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing using mainly spraying means, e.g. nozzles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus 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
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H01L21/67063—Apparatus for fluid treatment for etching
    • H01L21/67075—Apparatus for fluid treatment for etching for wet etching
    • H01L21/6708—Apparatus for fluid treatment for etching for wet etching using mainly spraying means, e.g. nozzles

Definitions

  • the present invention relates in general to an apparatus and method for cleaning surfaces, and in particular to the removal of organic films, particulate matter and other contaminants from surface of semiconductor wafers, with reduced residual impurities and contaminants.
  • Electrohydrodynamics create controlled-velocity nanodroplets that exhibit properties well-suited for such cleaning challenges.
  • Electrohydrodynamic atomization involves the use of a conducting fluid that is broken up and dispersed into a beam of charged nanodroplets. To initiate an EHD beam, an electrostatic stress is applied to a meniscus of the conducting fluid that exceeds the surface tension forces which hold the meniscus intact.
  • a small fluid reservoir holds a conductive process chemistry fluid to be sprayed, and an electrical contact in the reservoir applies a potential to the fluid.
  • a pneumatic controller applies a controlled pressure to the fluid in the reservoir, resulting in a flow of fluid from the reservoir, through a capillary tube, and into an electrostatic field at a spraying end of the capillary (or virtual nozzle).
  • EHD nanodroplet generation is controlled electrically, through reservoir charging levels and electric field manipulation at the nozzle. Speed and size of the nanodroplets can be varied, resulting in a wide range of process settings to match the nanodroplets to the contaminants and substrate. Nanodroplets can be created for ideal coupling of momentum transfer to particles.
  • EHD apparatus and method are described in U.S. Patent No. 6,033,484 entitled APPARATUS FOR CLEANING CONTAMINATED SURFACES USING ENERGETIC
  • CLUSTER BEAMS (Mahoney), the entire disclosure of which is hereby incorporated by reference, and U.S. Patent No. 5,796,111 entitled METHOD AND APPARATUS FOR CLEANING CONTAMINATED SURFACES USING ENERGETIC CLUSTER BEAMS (Mahoney), the entire content of which is hereby incorporated by reference.
  • electrosprayed liquids include water, alcohols (methanol, 2-propanol (IPA), ethanol), glycerol, hydroxylamine, n-methylpyrrolidone (NMP), and sulfuric acid.
  • the present invention is directed to a system and method for removing surface contaminants with electrosprayed beams of microdroplets, with reduced residual contaminants attributable to the microdroplets themselves.
  • the system and method may be used for cleaning surfaces, or even texturizing, etching or coating the surfaces.
  • the system includes a source configured to generate a beam of clusters to said surface, said source having an opening, a feed system configured to feed a liquid to said opening, and a treatment system configured to remove impurities from the liquid.
  • the source includes a device configured to generate an electric field to exert electrostatic forces higher than a surface tension of the liquid at the opening.
  • the treatment system includes a degasser to remove gases from the liquid, a filter to remove particulates from the liquid, and a pump to recirculate the liquid between the feed system and the treatment system.
  • the feed system includes a reservoir that is constructed of low particle shedding and chemically-resistant material, and the pump recirculates the liquid at a high volumetric flow rate that exceeds flow rate to the opening.
  • the system includes an electrode that charges the liquid.
  • the electrode may contain mono- atomic metallic elements, binary metallic alloys, tertiary metallic alloys, quaternary metallic alloys, and/or vitreous carbon, and selected chemistry between the electrode and the liquid can result in the formation of various species that can be effectively treated by the treatment system in reducing residual surface contaminants that are attributable to the electrosprayed liquid.
  • a method of the invention includes providing a source configured to generate a beam of clusters from an opening, feeding a liquid to the opening and removing impurities from the liquid, wherein the source generates an electric field to exert, electrostatic forces higher than a surface tension of the liquid at the opening.
  • removing impurities from the liquid comprises degassing the liquid, filtering the liquid and recirculating the liquid through a degasser and a filter.
  • the invention includes heating components, including an enclosure in which the beam of clusters are generated, providing electrostatic plates inside near the beam to attract ionic species within the beam, and/or facilitating condensation near the beam of gaseous species within the beam.
  • the enclosure can be heated to at least 150 degrees Centigrade for at least 30 minutes, and panels can be cooled cryogenically to facilitate condensation.
  • chemistry of the liquid and a charging electrode can be selected so that oxidation reactions at the electrode result in formation of gaseous products or insoluble layers that remain on the electrode rather than enter the solution.
  • the polarity of the voltage applied to the electrode can also affect the species that are formed.
  • FIG. 1 illustrates electrochemical reactions between a solution and an electrode within a reservoir of an EHD system.
  • FIG. 2 illustrates formation of a nanocluster from an EHD beam droplet.
  • FIG. 3 is a diagram showing an embodiment of a system in accordance with the present invention.
  • FIG. 3 a is a diagram showing an alternate embodiment of a system in accordance with the present invention.
  • the present invention recognizes that a source of contamination prior to atomization of an EHD sprayed solution involves droplets entrained with separated contaminant molecules that are introduced into the EHD solution through a variety of sources including contaminated starting solution, and particles shedding off containment members and conduits within an EHD apparatus. [0020] The present invention also recognizes that another source of contamination prior to atomization involves chemical interactions between the solution to be sprayed and the electrode that applies voltage and charges the solution. As illustrated in FIG. 1 , a solution 10 doped with a conductive additive AC is contained in an electrolytic cell or insulated reservoir 12. Adjoined paired molecules AC exist in the solution as non-disassociated electrolyte or solute molecules which form anion-cation pairs.
  • Adjoined paired molecules AC disassociate into solution anions A and solution cations C, either of which depending on the particular chemistry of the additive AC and the polarity of an immersed charging electrode 14 can interact with the material M of the electrode in forming new molecules MA or MC.
  • the new molecules are a volatile, gaseous species
  • the molecules rise harmlessly above the solution and can be pumped out.
  • the electrode/solution chemistry results in new molecules of a non-volatile species, they are transmitted by the solution to the nozzle providing a source of undesirable contaminants in the electrosprayed droplets. These non-volatile contaminants deposit on substrates that intercept the beam downstream of the atomization region.
  • the electrode material M is gold
  • the conductive additive is hydrochloric acid (HCL)
  • the gold electrode is connected to a source of positive voltage
  • AuCl molecular species result from electrolytic reactions between the electrode and the conductive additive, where the coalescence thereof within the droplets yield AuCl nanoclusters that are liberated after evaporation of in-flight beam droplets.
  • Electrode/electrolyte chemistry results in formation of nonvolatile, insoluble species that form insoluble layers that remain on the electrode rather than entering the solution.
  • the electrode is silver and the conductive additive is HCl, resulting molecular species AgCl that forms insoluble layers that remain on the electrode.
  • the present invention further recognizes that another source of contamination occurs after atomization where background gas molecules in an EHD process chamber can combine with the liquid beam droplets to create acidic material leading to surface residue.
  • contaminated EHD sprayed liquid or solution, used interchangeably herein
  • droplets 20 entrained with separated contaminant molecules 22 evaporates and shrinks in size, the molecules 22 coalesce into a non-volatile nanocluster 24.
  • the nanocluster 24 is liberated impacting substrate 26 and remains thereon as surface residual contaminant 28.
  • FIG. 3 an embodiment of a system 30 that generates a multiply charged electrosprayed beam consisting of droplets having nanometer and micrometer dimensions, with reduced surface residual contaminants is shown in FIG. 3.
  • a charged droplet beam 32 is generated by delivering a conductive solution 34 from a sealed, pressurized reservoir 36 along a capillary tube 38 to its an end or tip 40 (hereafter referred to as nozzle) having a small bore, preferably with a diameter in the range between about 25-100 microns, preferably between about 25 to 50 microns.
  • the tip 40, the capillary tube 38 and extractor electrodes 37 defining an electric field in an atomization region are collectively referred to an EHD droplet source 39.
  • the solution 34 which may be an organic or inorganic solution mixture is made conductive by addition of chemicals that impart electrolytic activity, for example, acids or bases.
  • the electrosprayed fluid can consist of a single component organic or inorganic liquid or a mixture of one or more chemically different components.
  • electrosprayed liquids include but are not limited to: hydrogen peroxide, TMAH, nitric acid, phosphoric acid, hydrofluoric acid and ammonium hydroxide.
  • TMAH hydrogen peroxide
  • nitric acid nitric acid
  • phosphoric acid phosphoric acid
  • hydrofluoric acid and ammonium hydroxide e.g., sodium bicarbonate
  • Many of the aforementioned chemicals can be combined in many ways to prepare solution mixtures sufficient to generate stable EHD beams.
  • the conductivity of the liquid may be too low or too high to achieve the desired beam properties of particle size and velocity. In these cases, amounts of added acidic or basic chemical agents are increased or lowered to achieve the desired beam properties.
  • the solution is charged by applying voltage to a conducting (metallic, carbon) wire or electrode 42 immersed in the solution 34. Applying pressure supplied by gas source 44, as regulated by pressure/flow controller 46, above the solution in the reservoir 36 causes the solution to flow through the capillary delivery tube 38.
  • the solution mixture Upon arrival at the nozzle 40 housed within an EHD process chamber 50 defined by a vacuum enclosure 52, the solution mixture is subjected to a high electrical field defined by the extractor electrodes 37 at atomization region 54 which disperses the charged liquid creating a beam of electrosprayed micron and submicron-sized droplets 32.
  • pre-spray management of solution electrolysis and post-spray management of the beam environment advantageously minimize if not avoid residue contaminant (defects) buildup on target substrate 56 during surface cleaning operations using apparatus 30.
  • the solution 34 contained in the reservoir 36 can be ultrapure with impurities at concentration levels of parts-per-billion or less.
  • Suitable starting solutions including chemical solutions from J.T. Baker sold under the trademark ULTREX, may be mixed with other solutions and/or electrolytes for use as the solution 34 in the reservoir 36.
  • the reservoir 36 is constructed of low particle shedding and chemically resistant materials, including PFA, TEFLON, PVDF, glass, and the like.
  • the apparatus 30 includes a treatment system 57 that in the embodiment of FIG. 3 includes a recirculating pump 58 that pumps, preferably continually, solution 34 through a degassing chamber or degasser 60 and an inline filtering unit 62 with a retention rating no greater than about 0.01 micron.
  • the filtering unit 62 returns filtered and outgassed solution back to the reservoir 36.
  • the degasser serves to eliminate dissolved gases from EHD process solutions that can act as precursors for droplet/particle nucleation.
  • Constant recycling of solution at high volumetric flow rates at the point-of-usage should minimize traces of particles and dissolved gases immediately prior to the low volumetric flow usage by EHD spraying at the nozzle.
  • Advantages are present when the recycling rate exceeds the usage rate or flow rate to the nozzle.
  • the recycling may be on the order of milliliter/min whereas the usage rate may be on the order of microliter/min.
  • the solution 34 exits the reservoir 36 through the capillary tube 38 and is delivered to the nozzle 40.
  • Flow of the solution through the capillary tube is regulated by the flow controller 46, using gas, for example, dry, ultrapure nitrogen gas, from gas source 44.
  • a filter 66 located between the gas source 44 and an input of the flow controller 46 removes particles from the gas, and a second filter 68 at the exit of the flow controller prevents particles that might originate in the flow controller or the gas source from entering the reservoir 36.
  • solution and electrode materials are peroxides, including hydrogen peroxide, in combination with an acid, including nitric acid, sulfuric acid and acetic acid, capable of disassociating in a polar solvent, such as water or glycerol, where a positive polarity is applied to a gold electrode, hi one embodiment, for example, the acid is nitric acid.
  • Solution and electrode materials are chosen so that oxidation reactions at the electrode result in formation of insoluble layers that remain on the electrode rather than enter the solution.
  • Any suitable acid may be used that is capable of disassociating in a polar solvent to form charged ions which are capable of forming a salt with the metal of the electrode that is insoluble in the polar solvent.
  • the electrode is any metal that can form a salt with a disassociated acid ion that is insoluble in a polar solvent.
  • using a silver electrode in the presence of HCl results in formation of silver chloride (AgCl) at the electrode with positive polarity which is insoluble in water or isopropanol (IPA).
  • the conducting electrode can be composed of different materials, including but not limited to:
  • a a mono-atomic metallic element, e.g., gold, silver, tantalum, platinum; [0037] b. any metallic alloy, including but not limited to binary, tertiary and quaternary metallic alloys; and [0038] c. vitreous carbons.
  • a mono-atomic metallic element e.g., gold, silver, tantalum, platinum
  • b any metallic alloy, including but not limited to binary, tertiary and quaternary metallic alloys
  • c vitreous carbons.
  • the solution as it arrives at the nozzle 40 for electrospraying should meet the following criteria:
  • the apparatus and method of the present invention minimizes background gases prior to and following initiation of the EHD spray.
  • the EHD process chamber 50 that is defined by a vacuum enclosure 52 into which the solution from the reservoir is delivered via the capillary tube upon increased pressurization above the solution in the reservoir, has heating components for heating the enclosure structure and cooling panels inside the chamber to facilitate collection by condensation of unwanted gaseous species arising from the electrosprayed liquid.
  • heater straps 70 are positioned outside the enclosure to heat the enclosure structure.
  • a method of treating an EHD process chamber to reduce substrate surface residual contaminants includes:
  • Acts A, B and C are initiated before initiation of electrospraying at the nozzle, although Acts B and C may be initiated after initiation of Act A 10 and/or after initiation of electrospraying at the nozzle. Moreover, Act B may be more effective than Acts C and A, and Act C may be more effective than Act A.

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  • 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

La présente invention concerne un système et un procédé utilisés pour éliminer des contaminants présents sur une surface au moyen de jets distribués par électronébulisation de microgouttes qui elles-mêmes ne laissent qu'une faible contamination résiduelle. Le système et le procédé peuvent être utilisés pour le nettoyage de surfaces ou même pour la texturation, la gravure ou le revêtement desdites surfaces. Dans un mode de réalisation, le système comprend une source conçue pour générer un faisceau d'agglomérats pour ladite surface, la source comportant une ouverture, un système d'alimentation configuré pour distribuer un liquide à ladite ouverture et un système de traitement conçu pour éliminer les impuretés du liquide. La source comprend un dispositif conçu pour générer un champ électrique capable d'exercer des forces électrostatiques supérieures à une tension superficielle du liquide au niveau de l'ouverture. Un procédé selon l'invention consiste à utiliser une source conçue pour générer un faisceau d'agglomérats par une ouverture, à alimenter l'ouverture en liquide et à éliminer les impuretés du liquide, ladite source générant un champ électrique qui exerce des forces électrostatiques supérieures à la tension superficielle du liquide au niveau de l'ouverture.
PCT/US2008/072038 2007-08-02 2008-08-01 Appareil faisant appel à des fluides électrostatiques distribués par électronébulisation pour nettoyer des surfaces, laissant une contamination résiduelle réduite et procédé correspondant WO2009032459A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US96343907P 2007-08-02 2007-08-02
US60/963,439 2007-08-02
US99370707P 2007-09-13 2007-09-13
US60/993,707 2007-09-13

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WO2009032459A1 true WO2009032459A1 (fr) 2009-03-12

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WO (1) WO2009032459A1 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20210077060A (ko) * 2019-12-16 2021-06-25 삼성디스플레이 주식회사 잉크젯 프린트 장치 및 쌍극자 정렬 방법

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5571385A (en) * 1995-05-08 1996-11-05 Cleveland State University Method and apparatus for water purification
US5653864A (en) * 1994-06-30 1997-08-05 Nok Corporation Protein biosensor and method for protein measurement with the same
US6033484A (en) * 1995-10-30 2000-03-07 Phrasor Scientific, Inc. Method and apparatus for cleaning contaminated surfaces using energetic cluster beams
US6106634A (en) * 1999-02-11 2000-08-22 Applied Materials, Inc. Methods and apparatus for reducing particle contamination during wafer transport
US6159421A (en) * 1995-10-17 2000-12-12 Ebara Corporation Method of cleaning gases
US20030015656A1 (en) * 2001-07-19 2003-01-23 Van Berkel Gary J. Thin-channel electrospray emitter
US6752860B1 (en) * 1999-06-28 2004-06-22 Statoil Asa Apparatus for separation of a fluid flow, especially into a gas phase and a liquid phase
US6953047B2 (en) * 2002-01-14 2005-10-11 Air Products And Chemicals, Inc. Cabinet for chemical delivery with solvent purging
US20060102471A1 (en) * 2004-11-18 2006-05-18 Karl Maurer Electrode array device having an adsorbed porous reaction layer
US20070009841A1 (en) * 2003-10-06 2007-01-11 Matsushita Electric Industrial Co., Ltd. Semiconductor fabrication apparatus and pattern formation method using the same

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5653864A (en) * 1994-06-30 1997-08-05 Nok Corporation Protein biosensor and method for protein measurement with the same
US5571385A (en) * 1995-05-08 1996-11-05 Cleveland State University Method and apparatus for water purification
US6159421A (en) * 1995-10-17 2000-12-12 Ebara Corporation Method of cleaning gases
US6033484A (en) * 1995-10-30 2000-03-07 Phrasor Scientific, Inc. Method and apparatus for cleaning contaminated surfaces using energetic cluster beams
US6106634A (en) * 1999-02-11 2000-08-22 Applied Materials, Inc. Methods and apparatus for reducing particle contamination during wafer transport
US6752860B1 (en) * 1999-06-28 2004-06-22 Statoil Asa Apparatus for separation of a fluid flow, especially into a gas phase and a liquid phase
US20030015656A1 (en) * 2001-07-19 2003-01-23 Van Berkel Gary J. Thin-channel electrospray emitter
US6953047B2 (en) * 2002-01-14 2005-10-11 Air Products And Chemicals, Inc. Cabinet for chemical delivery with solvent purging
US20070009841A1 (en) * 2003-10-06 2007-01-11 Matsushita Electric Industrial Co., Ltd. Semiconductor fabrication apparatus and pattern formation method using the same
US20060102471A1 (en) * 2004-11-18 2006-05-18 Karl Maurer Electrode array device having an adsorbed porous reaction layer

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