EP2269208B1 - Appareil et procédés pour une utilisation d'agents anti-adhérents réfractaires dans la protection de feuilles et de fils métalliques - Google Patents

Appareil et procédés pour une utilisation d'agents anti-adhérents réfractaires dans la protection de feuilles et de fils métalliques Download PDF

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Publication number
EP2269208B1
EP2269208B1 EP09739151A EP09739151A EP2269208B1 EP 2269208 B1 EP2269208 B1 EP 2269208B1 EP 09739151 A EP09739151 A EP 09739151A EP 09739151 A EP09739151 A EP 09739151A EP 2269208 B1 EP2269208 B1 EP 2269208B1
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EP
European Patent Office
Prior art keywords
refractory
foil
abhesive
pinch
metallic foil
Prior art date
Legal status (The legal status 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 status listed.)
Not-in-force
Application number
EP09739151A
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German (de)
English (en)
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EP2269208A1 (fr
EP2269208A4 (fr
Inventor
Tryggvi Emilsson
Nikolaus Voggenauer
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Advanced Lighting Technologies Inc
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Advanced Lighting Technologies Inc
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Publication date
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Publication of EP2269208A1 publication Critical patent/EP2269208A1/fr
Publication of EP2269208A4 publication Critical patent/EP2269208A4/fr
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Publication of EP2269208B1 publication Critical patent/EP2269208B1/fr
Not-in-force legal-status Critical Current
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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/02—Details
    • H01J61/36—Seals between parts of vessels; Seals for leading-in conductors; Leading-in conductors
    • H01J61/366—Seals for leading-in conductors
    • H01J61/368—Pinched seals or analogous seals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/02—Details
    • H01J61/30—Vessels; Containers
    • H01J61/34—Double-wall vessels or containers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
    • H01J9/32—Sealing leading-in conductors
    • H01J9/323—Sealing leading-in conductors into a discharge lamp or a gas-filled discharge device
    • H01J9/326—Sealing leading-in conductors into a discharge lamp or a gas-filled discharge device making pinched-stem or analogous seals

Definitions

  • the present subject matter generally relates to electrical lead assemblies in devices such as electric lamps for providing an electrical path through a hermetic press, pinch, or shrink seal formed in a vitreous material such as fused silica or hard glass.
  • a light emitting chamber is formed from a vitreous material having one or more pinch seals that hermetically seal the chamber.
  • one or more electrically-conducting paths from the interior of the chamber to the exterior of the chamber are typically formed by positioning an electrical assembly in one or more of the portions of the tube, and "pinching" the tube to form a hermetic seal around a portion of the assembly.
  • the electrical lead assembly typically includes a metallic foil having electrically conducting leads mechanically secured to the foil and extending from each end thereof.
  • the assembly is positioned so that the foil forms the electrically conducting path through a portion of the vitreous material that has been pinched or shrunk together to form a hermetic seal.
  • the foil in such electrical lead assemblies is formed from molybdenum because of its stability at high temperatures, relatively low thermal expansion coefficient, good ductility, and sufficient electrical conductivity.
  • molybdenum oxidizes rapidly when exposed to oxygen at temperatures greater than about 350°C.
  • the foils in electrical lead assemblies in electric lamps are often exposed to temperatures greater than about 350°C, the metallic foil may be highly susceptible to oxidation resulting in a breach of the electrical path or the gas-tight integrity of the hermetic seal resulting in lamp failure.
  • a molybdenum foil exposed to a reactive atmosphere will not oxidize appreciably below about 350°C.
  • the rate of the reaction between the oxygen in the surrounding atmosphere and the molybdenum foil greatly increases resulting in corrosion of the foil and a substantial reduction in the useful life of the lamp.
  • Areas particularly susceptible to such oxidation include the spot weld connecting the outer lead to the foil and the area on the foil adjacent the outer lead.
  • FIG 1a is a schematic representation of a conventional arc tube for a high intensity discharge lamp.
  • the arc tube 100 is formed from light transmissive material such as quartz.
  • the arc tube 100 defines a chamber 110 formed by pinch sealing the end portions 115, 120.
  • An electrode assembly 122, 124 is sealed within each end portion 115, 120 to provide an electrically-conducting path from the interior of the chamber 110 to the exterior of the chamber through each end portion 115, 120.
  • Each electrode assembly 122, 124 for a high intensity discharge arc tube 100 typically includes a discharge electrode 125, 130, electrode leads 140, 135, metallic foils 145, 150, and outer leads 155, 160.
  • the electrode leads 135, 140 and the outer leads 155, 160 are typically connected to the metallic foils 145, 150 by spot welds.
  • Figure 1b is an illustration of the cross-section of a typical metallic foil 145, 150 in an electrical lead assembly 122, 124.
  • the typical foil 145, 150 is shaped in cross-section so that the thickness of the foil is greatest at the lateral center thereof, and reduces outwardly to each of the longitudinal edges. This shape has been found to reduce residual strain in the vitreous material that has been compressed around the foil during the high temperature pinching process and subsequently cooled.
  • the foil may have a width of about 2 to 5.5 mm with a centerline thickness of about 20 to 50 ⁇ m and an edge thickness of about 3 to 7 ⁇ m.
  • a foil having a width of about 2.5 mm would typically have a centerline thickness of about 24-25 ⁇ m and an edge thickness of about 3 ⁇ m.
  • the assemblies 122, 124 are positioned in the end portions 115, 120 so that the foils 145, 150 are pinched between the compressed portions of the end portions 115, 120 forming the hermetic pinch seals.
  • the assemblies 122, 124 provide the electrically conducting paths through the each end portion 145, 150 with the relatively thin foils 145, 150 providing a current path through the hermetically sealed pinch regions.
  • the electrode lead assemblies provide a point of failure in such lamps due to corrosion, e.g., oxidation, of the metallic foils when exposed to corrosive agents such as oxygen at high temperatures.
  • corrosion e.g., oxidation
  • the assemblies 122, 124 are particularly susceptible to oxidation at the outer portion of the foil 145, 150 adjacent the outer lead 155, 160 due to the exposure of this portion of the foil to oxygen or other corrosive agents during operation of the lamp.
  • the oxidation may progress inward placing a significant amount of stress on the pinch seal. The stress may be evident from Newton rings or passageways which appear at the point at which the leads are welded to the molybdenum foil. Eventually, the electrical path may be breached or the pinch seal may crack causing the lamp to fail.
  • Another reason for this failure may also be the result of two mechanisms.
  • Efforts have been made in the past to prevent the oxidation of molybdenum foils in electrical assemblies that may be exposed to oxygen at high temperatures. For example, it has been proposed to reduce oxidation by coating the molybdenum foil with oxidation-protective materials such as phosphides ( U.S. Pat. No. 5,387,840 ), aluminides, lead oxide, silicon nitride, alkali metal silicate and chromium ( U.S. Pat. No. 3,793,615 ).
  • Another conventional practice for protecting the molybdenum foil involves filling the open end of the pinch or shrink area with a low-melting antimony borate glass.
  • Yet another conventional practice includes protecting the outer lead with a platinum cladding.
  • Pinch seal assemblies comprising metal foils coated with powders of refractory metals are disclosed e.g. by US3693241 and GB671178 .
  • the utility of the aforementioned prior art approaches are marginally adequate and/or expensive; however, none of these prior art approaches includes the application of glassy films.
  • the present invention provides a device according to the subject-matter of claim 1 and a method according to the subject-matter of claim 7.
  • Figure 1a is a schematic representation of a conventional arc tube for a high intensity discharge lamp.
  • Figure 1b is an illustration of a prior art metallic foil in cross-section.
  • Figure 2 is a schematic representation of an arc tube.
  • Figure 3 is a schematic representation of a formed body arc lamp for a high intensity discharge lamp.
  • Figure 4 is a schematic representation of another formed-body high intensity discharge lamp.
  • Figure 5 is a schematic representation of a high intensity discharge lamp showing a mechanical support of arc tube and wrapped/crimped electrical connections to foil.
  • Figure 6 is a representation of subject matter.
  • a metallic foil may be coated to inhibit corrosion and the method for applying such coating.
  • a foil is particularly advantageous in electrical lead assemblies because the foil may form the outer lead in the assembly and may extend beyond the end portion of the arc tube, thus eliminating the relatively thicker wire outer lead.
  • a method for protecting metallic foils in electrical lead assemblies from corrosion is provided by coating the foil with a silica film, refractory abhesive and/or combination thereof.
  • the coating provides a barrier for the foil to oxygen and other corrosive agents at high temperatures, thus reducing the corrosion of the foil and eliminating a significant cause of premature failure in electric lamps.
  • Another method for coating metallic foil by immersing at least a portion of the foil in a bath of colloidal silica and/or silica-abhesive slurry, withdrawing the foil from the bath at a controlled rate so that silica colloid adheres to the foil, and exposing the silica colloid to a temperature sufficient to effect fusion of silica particles thereby forming a thin film of silica on the foil.
  • a bath of colloidal silica and/or silica-abhesive slurry withdrawing the foil from the bath at a controlled rate so that silica colloid adheres to the foil, and exposing the silica colloid to a temperature sufficient to effect fusion of silica particles thereby forming a thin film of silica on the foil.
  • Patent Application No. 11/545,469 which is a divisional application of U.S. Patent No. 7,153,179 ; however, other methods of applying the coating to the foil may be used.
  • the coating may be applied by electrostatic spray coating, dipping, rolling, brushing and misting.
  • Another techniques for applying the coating may include adding fine silica powder to the plume of an argon plasma torch thereby producing a spray of liquid silica.
  • silica coated structures When silica coated structures are sealed into fused vitreous material such as quartz, the coatings adhere to the vitreous material since they are the same material. Upon cooling and thermal contraction, the protective coating may peel or strip off the metal and severe shaling of the glass may be observed. Through an application of a refractory abhesive to the silica coated structures, the fused vitreous material does not adhere, and the integrity of the protective coat may be maintained.
  • Exemplary refractory abhesive materials may be, but are not limited to, boron nitride, graphite, powders or flakes of refractory metals (such as Tungsten, Tantalum, Hafnium, Niobium, Rhenium, Osmium, etc.), or powders or flakes of refractory oxides (such as Yttrium Oxide, Zirconium Oxide, Thorium Oxide, Magnesium Oxide, Beryllium Oxide, etc.).
  • the application of refractory abhesive materials to embodiments of the present subject matter may also prevent shaling of the silica glass caused by adherence to metal parts during pinching.
  • refractory abhesives may improve the life of a pinch or shrink seal and hence the respective arc tube or lamp by preventing the weakening of the vitreous material and by reducing the oxidation of the metal (e.g ., slowing the access of air to the vulnerable metal).
  • the permeability to air may be further decreased by fusible additives in the refractory abhesive formulation that promotes bonding of the refractory abhesive particles to each other and to the metal.
  • additional protection of the foils and outer lead wires in electrical lead assemblies of electric lamps may also be achieved by mixing colloidal silica with a refractory abhesive slurry. This mixture may be applied to the assemblies by dipping, spraying, or any other suitable method. When the assembly is pinched or shrunk, the silica fuses, covering the metal with liquid silica and trapping the refractory abhesive particles in a silica matrix. Upon cooling of the assembly, the silica may remain bonded to the metal and any thermally induced cracking may occur within the silica-abhesive layer.
  • silica-abhesive e.g ., silica-boron nitride, etc.
  • silica-boron nitride may react chemically with the metal to produce coatings of materials having exceptional oxidation protective properties.
  • certain mixtures of silica-boron nitride causes a melting of the molybdenum surface and creates a layer of a substance highly resistant to oxidation. In this example, the layer appears to be a molybdenum boride.
  • compositions of silica-abhesives may be equally effective, and such an example should not limit the scope of the claims appended herewith.
  • FIG. 2 is a schematic representation of a pinched tube.
  • outer leads in the assemblies are eliminated by extending the length of the foil.
  • the outer leads may be eliminated from the assembly.
  • This set-up has the additional advantage of eliminating the need to adhere (spot weld, mechanical attachment, etc.) the outer leads to the foil. This will enhance the life of the lamp by avoiding the capillary formation or other such voids in the pinch seal. Further enhancement of the life of the lamp may be provided by coating any portion(s) of the foils 113, 150, 155 with an exemplary refractory abhesive or a silica-abhesive coating described above.
  • an arc tube 300 may include the chamber 110 and the end portions 115, 120 that are sealed by pinching.
  • the lead assemblies may include electrode leads 135, 140, foils 145, 150, and outer leads 155, 160. Enhancement of the life of the arc tube 300 may be provided by coating any portion(s) of the end portions 115, 120 and/or the lead assemblies including the electrode leads 135, 140, foils 145, 150 and outer leads 155, 160 with an exemplary refractory abhesive or a silica-abhesive coating described above.
  • each of foils 150, 155 may be extended beyond the respective end portions 115, 120 of the arc tube 400 thereby eliminating the outer leads from the assemblies.
  • enhancement of the life of the arc tube 400 may be provided by coating any portion(s) of the end portions 115, 120 and/or foils 150, 155 with an exemplary refractory abhesive or a silica-abhesive coating described above.
  • FIG. 5 is a schematic representation of a high intensity discharge lamp showing a mechanical support for arc tube and wrapped/crimped electrical connections to the foil.
  • High intensity discharge lamp 500 includes an arc tube 505 supported with the outer lamp envelope 508 of the lamp 500.
  • the arc tube 505 includes a bulbous chamber 510 intermediate tubular end portions 512, 514.
  • the arc tube 505 is mechanically secured within the envelope by supporting the arc tube at the end portions 512, 514 thereof.
  • the electrical assemblies of the arc tube include metallic foils 515, 525 that extend beyond the end portions 512, 514 to provide electrical connections for the arc tube.
  • the electrical leads connecting the lamp base to the foils are mechanically and electrically secured to the foils by coil connections 527, 528.
  • the foils 515, 525 are not as mechanically rigid as the outer leads in conventional lead assemblies, mechanical deformation of the foils is minimized by supporting the arc tube 505 from the end portions 512, 514. Enhancement of the life of the arc tube 500 may be provided by coating any portion(s) of the electrical assemblies of the arc tube 500 including the foils 515, 525 with an exemplary refractory abhesive or a silica-abhesive coating described above.
  • a method 600 of providing an electrical connection through a pinch or shrink seal formed in a quartz or glass body is illustrated.
  • a quartz or glass body having at least one open end is provided, and at step 620, an electrical lead assembly comprising a metallic foil is also provided.
  • the metallic foil may be formed from molybdenum, however, such an example should not limit the scope of the claims appended herewith as the metallic foil may be formed from any suitable metal or material.
  • a coating comprising a refractory abhesive may be applied to at least a portion of the metallic foil.
  • the refractory abhesive may be, but is not limited to, boron nitride, graphite, powders or flakes of refractory metals, and powders or flakes of refractory oxides.
  • the application of the refractory abhesive may include mixing colloidal silica with a refractory abhesive slurry and applying the mixture to at least a portion of the metallic foil.
  • the electrical lead assembly may be positioned in an open end of the body at step 640, and the open end of the body may be pinch or shrink sealed so that the quartz or glass of the body forms a hermetic seal around the metallic foil of the electrical lead assembly at step 650.
  • the assemblies were overcoated with an exemplary refractory abhesive, specifically, (1) graphite (TC-2 from Fiber Materials, Inc.) diluted 1:1 with amyl acetate, and (2) boron nitride (BN Aerosol Brushable, Zyp Coatings).
  • graphite TC-2 from Fiber Materials, Inc.
  • boron nitride BN Aerosol Brushable, Zyp Coatings
  • the assemblies were overcoated with an exemplary refractory abhesive only up to the outer lead weld.
  • the refractory abhesives were (1) graphite (TC-2 from Fiber Materials, Inc.) diluted 1:1 with amyl acetate, and (2) boron nitride (BN Aerosol Brushable, Zyp Coatings).
  • TC-2 from Fiber Materials, Inc.
  • boron nitride BN Aerosol Brushable, Zyp Coatings
  • Pieces of molybdenum foil and/or lead junctions and weld spots of bare assemblies, having no silica coatings were provided with a refractory abhesive coating, namely, boron nitride. Boron nitride coatings were also applied to the electrode shank/foil junctions.
  • the refractory abhesive coatings provided no negative impact on the internal lamp operating characteristics. In comparison, lamps made with bare foil/lead assemblies illustrated a typical failure within 500 hours of operation; however, lamps made with the exemplary refractory abhesive coating of boron nitride exhibited no oxidation damage at 500 hours of operation.
  • Pieces of molybdenum foil and/or lead junctions and weld spots of bare assemblies, having no silica coatings were provided with a refractory abhesive coating, namely, a mixture of silica and boron nitride.
  • a refractory abhesive coating namely, a mixture of silica and boron nitride.
  • Exemplary lamps made with this refractory abhesive coating exhibited excellent oxidation protection at 400°C for several thousand hours of operation.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Vessels And Coating Films For Discharge Lamps (AREA)
  • Manufacture Of Electron Tubes, Discharge Lamp Vessels, Lead-In Wires, And The Like (AREA)

Claims (11)

  1. Dispositif comprenant:
    un corps en quartz ou en verre formant une chambre et possédant un ou plusieurs joints à pincement ou rétractables formés dans le corps ; et
    un assemblage de fils électriques adapté pour fournir une connexion électrique par le biais d'un joint à pincement dans un corps en quartz ou en verre, ledit assemblage comprenant une feuille métallique possédant un revêtement sur au moins une partie de celle-ci comprenant un agent anti-adhérent réfractaire ; dans lequel l'agent anti-adhérent réfractaire est un matériau ayant la capacité de résister à l'adhérence au corps en quartz ou en verre et est choisi dans le groupe constitué du nitrure de bore, du graphite, des poudres ou des paillettes de métaux réfractaires, et des poudres ou des paillettes d'oxydes réfractaires ;
    dans lequel la feuille métallique est positionnée à l'intérieur du joint à pincement ou rétractable, et caractérisé en ce que ledit revêtement comprend également de la silice colloïdale.
  2. Dispositif selon la revendication 1 dans lequel ladite feuille métallique est fabriquée à partir de molybdène.
  3. Dispositif selon la revendication 1 ou 2 dans lequel ledit agent anti-adhérent réfractaire comprend du nitrure de bore.
  4. Dispositif selon l'une quelconque des revendications précédentes comprenant un film sur au moins une partie de ladite feuille, ledit film comprenant un composé contenant un métal de ladite feuille.
  5. Dispositif selon la revendication 4 dans lequel la feuille métallique est fabriquée à partir de molybdène et ledit film comprend un composé de molybdène.
  6. Dispositif selon la revendication 5 dans lequel ledit composé de molybdène est fabriqué par réaction chimique entre un ou plusieurs éléments dudit revêtement et de ladite feuille.
  7. Procédé servant à créer une connexion électrique par le biais d'un joint à pincement ou rétractable formé dans un corps en quartz ou en verre, ledit procédé comprenant :
    la fourniture d'un corps en quartz ou en verre possédant au moins une extrémité ouverte ;
    la fourniture d'un assemblage de fils électriques comprenant une feuille métallique ;
    l'application d'un revêtement comprenant une silice colloïdale et un agent anti-adhérent réfractaire sur au moins une partie de la feuille métallique, dans lequel l'agent anti-adhérent réfractaire est un matériau ayant la capacité de résister à l'adhérence au corps en quartz ou en verre et est choisi dans le groupe constitué du nitrure de bore, du graphite, des poudres ou des paillettes de métaux réfractaires et des poudres ou des paillettes d'oxydes réfractaires ;
    le positionnement de l'assemblage de fils électriques dans une extrémité ouverte du corps ;
    la fermeture par pincement ou rétraction de l'extrémité ouverte du corps de manière à ce que le quartz ou le verre du corps forme un joint hermétique autour de la feuille métallique de l'assemblage de fils électriques.
  8. Procédé selon la revendication 7 dans lequel la feuille métallique est fabriquée à partir de molybdène.
  9. Procédé selon les revendications 7 ou 8 dans lequel l'étape consistant à appliquer un revêtement comprenant un agent anti-adhérent réfractaire sur au moins une partie de la feuille métallique comprend le mélange de ladite silice colloïdale avec une suspension concentrée d'agent anti-adhérent réfractaire et l'application du mélange sur au moins une partie de la feuille métallique.
  10. Procédé selon l'une des revendications 7 à 9, dans lequel l'étape consistant à appliquer un revêtement comprend :
    l'application d'une couche de protection comprenant des précurseurs de verre fusibles sur au moins une partie de l'assemblage de fils électriques ;
    l'application d'une couche de matériau sur au moins une partie de la couche de protection, le matériau étant adapté pour prévenir l'adhérence de la couche de protection recouverte par le matériau et le corps en verre lorsque l'assemblage de fils électriques est enfermé hermétiquement à l'intérieur d'un joint à pincement ou rétractable dans le corps.
  11. Procédé selon l'une des revendications 7 à 9, dans lequel l'étape consistant à appliquer un revêtement comprend : l'application d'une couche de protection sur au moins une partie de l'assemblage de fils électriques, la couche de protection comprenant des précurseurs de verre fusibles et un matériau qui prévient mécaniquement la forte adhérence de la couche de protection au corps en verre lorsque l'assemblage de fils électriques est enfermé hermétiquement à l'intérieur d'un joint à pincement ou rétractable dans le corps.
EP09739151A 2008-04-28 2009-04-28 Appareil et procédés pour une utilisation d'agents anti-adhérents réfractaires dans la protection de feuilles et de fils métalliques Not-in-force EP2269208B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US7141708P 2008-04-28 2008-04-28
PCT/US2009/002573 WO2009134348A1 (fr) 2008-04-28 2009-04-28 Appareil et procédés pour une utilisation d’agents anti-adhérents réfractaires dans la protection de feuilles et de fils métalliques

Publications (3)

Publication Number Publication Date
EP2269208A1 EP2269208A1 (fr) 2011-01-05
EP2269208A4 EP2269208A4 (fr) 2011-08-31
EP2269208B1 true EP2269208B1 (fr) 2013-03-20

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EP09739151A Not-in-force EP2269208B1 (fr) 2008-04-28 2009-04-28 Appareil et procédés pour une utilisation d'agents anti-adhérents réfractaires dans la protection de feuilles et de fils métalliques

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EP (1) EP2269208B1 (fr)
JP (1) JP2011519138A (fr)
CN (1) CN101981648B (fr)
WO (1) WO2009134348A1 (fr)

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US707723A (en) * 1902-01-20 1902-08-26 Frank A Robbins Combination-tool.
DE821079C (de) * 1949-07-01 1951-11-15 Lumalampan Ab Folieneinschmelzung fuer elektrische Lampen in Quarz
US3693241A (en) * 1970-08-27 1972-09-26 Elmer G Fridrich Manufacture of foil seals
GB1521129A (en) * 1976-11-11 1978-08-16 Gen Electric Co Ltd High pressure electric discharge lamps
JPS61206243A (ja) * 1985-03-08 1986-09-12 Mitsubishi Electric Corp 高融点金属電極・配線膜を用いた半導体装置
US5310476A (en) * 1992-04-01 1994-05-10 Moltech Invent S.A. Application of refractory protective coatings, particularly on the surface of electrolytic cell components
US5754005A (en) * 1993-10-29 1998-05-19 General Electric Company Electric lamps containing electrical leads of a molybdenum and tungsten alloy
US5536991A (en) * 1994-09-13 1996-07-16 General Electric Company Lamp having silica protective coating

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Publication number Publication date
EP2269208A1 (fr) 2011-01-05
EP2269208A4 (fr) 2011-08-31
WO2009134348A1 (fr) 2009-11-05
CN101981648A (zh) 2011-02-23
CN101981648B (zh) 2014-07-09
JP2011519138A (ja) 2011-06-30

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