EP1899277A1 - Agent de gravure de couches conductrices transparentes oxydantes - Google Patents

Agent de gravure de couches conductrices transparentes oxydantes

Info

Publication number
EP1899277A1
EP1899277A1 EP06754211A EP06754211A EP1899277A1 EP 1899277 A1 EP1899277 A1 EP 1899277A1 EP 06754211 A EP06754211 A EP 06754211A EP 06754211 A EP06754211 A EP 06754211A EP 1899277 A1 EP1899277 A1 EP 1899277A1
Authority
EP
European Patent Office
Prior art keywords
etching
iii
iron
chloride
acid
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.)
Withdrawn
Application number
EP06754211A
Other languages
German (de)
English (en)
Inventor
Werner Stockum
Armin Kuebelbeck
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Merck Patent GmbH
Original Assignee
Merck Patent GmbH
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 Merck Patent GmbH filed Critical Merck Patent GmbH
Publication of EP1899277A1 publication Critical patent/EP1899277A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Definitions

  • the present invention relates to a novel dispensable homoge- neous etch medium with non-Newtonian flow behavior for etching oxidic transparent conductive layers and the use thereof, for example for the production of liquid crystal displays (LCD) or organic light emitting displays (OLED). Specifically, they are particle-free compositions that selectively etch fine structures into oxidic transparent and conductive layers without damaging or attacking adjacent surfaces.
  • LCD liquid crystal displays
  • OLED organic light emitting displays
  • An LC display consists essentially of two with oxidic transparent conductive layers, usually indium tin oxide (ITO), provided glass plates, between which there is a liquid crystal layer, which change their light transmission by applying a voltage.
  • ITO indium tin oxide
  • spacers prevents the touch of the ITO front and back.
  • the glass sheets used for the display production usually have a one-sided ITO layer thickness in the range of 20 to 200 nm, in most cases in the range of 30 to 130 nm.
  • the transparent conductive layer on the glass panes is structured in several process steps.
  • the method of photolithography known to those skilled in the art is used.
  • inorganic surfaces are understood as meaning oxidic compounds which have an increased electrical conductivity and retention of optical transparency by addition of a dopant.
  • the layer systems known to the person skilled in the art are omitted:
  • ITO layers having a sufficient conductivity by wet-chemical coating (Sol-GeI dip method) using a liquid or dissolved solid presursor in a solvent or solvent mixture.
  • These liquid compositions are usually applied by spin coating on the substrate to be coated.
  • the person skilled in the art is aware of these compositions as spin-on-glass systems (SOG).
  • etchants i. Of chemically aggressive compounds it comes to the dissolution of the attack of the etchant exposed material. In most cases, the goal is to completely remove the layer to be etched. The end of the etching is achieved by hitting a layer which is largely resistant to the etchant.
  • Photolithography involves material-intensive, time-consuming and costly process steps: According to known processes, the following steps are required for producing a negative or positive of the etching structure (depending on the photoresist):
  • Coating of the substrate surface eg by centrifugal coating with a liquid photoresist
  • drying of the photoresist exposure of the coated substrate surface
  • development, rinsing if necessary drying of the structures
  • etching of the structures for example by dipping methods (eg wet etching) in wet-chemical benches)
  • the etching solution is applied to a rotating substrate, the etching can be done without / with energy input (e.g., IR or UV irradiation) o dry etching method such as e.g. Plasma etching in complex vacuum systems or etching with reactive gases in
  • the laser beam scans the areas to be removed point by point or line by line in a vector-oriented system.
  • the transparent conductive layer is spontaneously vaporized by the high energy density of the LASER beam.
  • the method is quite well suited for structuring simple geometries. It is less suitable for more complex structures and especially for the removal of larger areas of transparent conductive layers. in this connection - A -
  • the LASER structuring is in principle poorly suited: evaporating transparent conductive material deposits in the immediate vicinity of the substrate and increases the thickness of the transparent conductive coating in these edge regions , This is a considerable problem for the further process steps, in which a surface that is as flat as possible is required.
  • compositions suitable for solving the problem of the invention in the form of pastes By attempts to produce compositions suitable for solving the problem of the invention in the form of pastes, it has been found that comparable printing and dispensing properties can be achieved through the use of selected thickeners as with particle-containing pastes. It can be formed by chemical interactions with the other components of the etching medium, a gel-like network. These new gel-like pastes exhibit particularly excellent paste application properties via dispenser technology, enabling contactless paste application.
  • the object of the invention selectively surfaces of oxide layers, in particular of tin or zinc oxide layers or corresponding doped layers, such as indium-tin oxide ln 2 O 3 : Sn (ITO), fluorine-doped tin oxide SnO 2 : F (FTO), antimony-doped tin oxide SnO 2 : Sb (ATO) or aluminum-doped zinc oxide ZnO: Al (AZO), to etch or structure is surprisingly by use of ferric (III) chloride or iron (III) chloride hexahydrate as a corrosive component for corresponding oxidic Surfaces solved.
  • the solution of the object of the invention in the provision and use of a new printable etching medium preferably with non-Newtonian flow behavior in the form of an etching paste for etching doped oxide, transparent conductive layers.
  • a corresponding paste contains thickeners selected from the group consisting of polystyrene, polyacrylic, polyamide, polyimide, polymethacrylate, melamine, urethane, benzoguanine, phenolic resin, silicone resin, fluorinated polymers (PTFE, PVDF, etc.), and micronized wax, in the presence of at least a caustic component, as well as at least one solvent.
  • the composition according to the invention may contain inorganic and / or organic acid and, if appropriate, additives such as defoamers, thixotropic agents, leveling agents, deaerators, adhesion promoters.
  • Compositions are to be activated at ehöhtenTemperaturen in the range 30-330 0 C, preferably in the range of 40 to 200 0 C and most preferably 50 to 120 0 C effective or can be prepared by introduction of energy in form of heat or IR-radiation.
  • the solution of the object according to the invention by the use of iron (III) chloride or iron (III) chloride hexahydrate as a selectively etching component in compositions in the form of pastes according to claims 2-7 for etching of oxidic surfaces, in particular for Etching of surfaces consisting of SnO 2 or zinc oxide or of oxidic, transparent, conductive layers which, in addition to SnO 2 or zinc oxide optionally contain one or more doping components, or for etching uniform, massive, non-porous or porous doped tin oxide surfaces, (ITO and / or FTO) systems as well as variable thickness layers of such systems.
  • pastes having the properties claimed in claim 8 are used to etch these surfaces.
  • Preferred for the claimed uses are compositions according to claims 12-23.
  • the present application moreover also relates to the use of iron (III) chloride or iron (III) chloride hexahydrate-containing compositions for the etching of SiO 2 or silicon nitride-containing glasses and of the above-mentioned oxidic surfaces in particular industrial production process according to claims 9 - 11.
  • oxidic surfaces can be selectively and easily etched using a composition containing iron (III) chloride or iron (III) chloride hexahydrate as the etching component.
  • Particularly suitable are those compositions for surfaces containing or consisting of SnO 2 or zinc oxide. Thin lines and finest
  • Structures can be etched with these compositions into oxidic, transparent, conductive layers which, in addition to SnO 2 or zinc oxide, contain one or more doping components.
  • these compositions can also be used excellently for etching uniform, massive, nonporous or porous doped tin oxide surfaces, (ITO and / or FTO) systems and layers of variable thickness of such systems.
  • Particularly good etching results are achieved when iron (III) chloride or iron (III) chloride hexahydrate is used as described as a caustic component in a composition for etching oxide surfaces in the presence of an inorganic mineral acid, wherein a mineral acid selected from the group of US Pat Group hydrochloric acid, phosphoric acid, sulfuric acid and nitric acid is used.
  • Iron (III) chloride or iron (III) chloride hexahydrate can in this case be selected in the presence of a mineral acid and / or at least one organic acid which may have a straight-chain or branched alkyl radical having 1-10 C atoms, selected from among Group of alkylcarboxylic acids, hydroxycarboxylic acids or dicarboxylic acids are used. Particularly suitable for this purpose are organic acids selected from the group consisting of formic acid, acetic acid, lactic acid and oxalic acid.
  • compositions in the form of a paste which comprise homogeneously distributed thickeners in an amount of from 0.5 to 25% by weight included on the total.
  • Thickeners may be one or more homogeneously dissolved thickeners from the group consisting of cellulose / cellulose derivatives and / or starch / starch derivatives and / or xanthan and / or polyvinylpyrollidone,
  • Advantageous properties for the use according to the invention have corresponding pastes, which at 20 0 C has a viscosity in a range of 6 to 35 Pa ⁇ s at a shear rate of up to 25 s ' 1 , preferably a viscosity in the range of 10 to 25 Pa * s and more particularly in the range of 15 to 20 Pa ⁇ s exhibit.
  • Such etch pastes are eminently suitable for etching SiO 2 or silicon nitride containing glasses that exist as uniform solid nonporous and porous solids or for etching corresponding nonporous and porous glass layers of variable thickness that have been formed on other substrates.
  • the paste-like compositions are also readily applicable to the opening of layers of doped tin oxide surfaces (ITO and / or FTO) in the fabrication process of semiconductor devices and their circuits or components for high power electronics and result in very accurate etch results.
  • Special applications are possible for the compositions containing iron (III) chloride or iron (III) chloride hexahydrate in the form of pastes in display technology (TFT), in photovoltaics, semiconductor technology, high-performance electronics, mineralogy or the glass industry, in Production of OLED lighting, of OLED displays, as well as in the production of photodiodes and for structuring of ITO glasses for flat screen applications (plasma displays).
  • the compositions for etching oxidic layers contain a) iron (III) chloride or iron (III) chloride hexahydrate as corrosive
  • additives such as defoamers, thixotropic agents, leveling agents, deaerators, adhesion promoters, and are in the form of pastes which are printable are and can be applied by appropriate printing techniques in thinnest lines or finely structured on the surfaces to be etched.
  • compositions may contain the etching component in an amount of 1 to 30% by weight and the thickener in an amount of 3 to 20% by weight based on the total amount.
  • the etching component is contained in an amount of 2 to 20 wt .-%, particularly preferably in an amount of 5 to 15 wt .-%, based on the total amount.
  • compositions except iron (III) chloride or iron (III) chloride hexahydrate as corrosive component an inorganic mineral acid selected from the group of hydrochloric acid, phosphoric acid, sulfuric acid, nitric acid and / or at least one organic acid which may have a straight-chain or branched alkyl radical having 1-10 C atoms selected from the group of the alkylcarboxylic acids containing hydroxycarboxylic acids or dicarboxylic acid solutions, since the etching process thereby meets the requirements of the respective US Pat to adapt to corrosive layers.
  • organic acids formic acid, acetic acid, lactic acid and oxalic acid are particularly suitable for the preparation of the pastes according to the invention.
  • the proportion of organic and / or inorganic acid (s) in a concentration range from 0 to 80 wt .-% based on the total amount of the medium, wherein the added acid or mixtures thereof each have a pK s value between 0 to 5 own.
  • the compositions of the invention water, monohydric or polyhydric alcohols selected from the group glycerol, 1.2 propanediol, 1, 4-butanediol, 1, 3-butanediol, 1, 5- Q pentanediol, 2-ethyl-1-hexenol, ethylene glycol , Diethylene glycol and dipropylene glycol, ethers selected from the group consisting of ethylene glycol monobutyl ether, triethylene glycol monomethyl ether, diethylene glycol monobutyl ether and dipropylene glycol monomethyl ether, esters selected from the group consisting of 2,2-butoxy- (ethoxy) -ethyl acetate, propylene carbonate, and 5- ketones, such as acetophenone, methyl 2-hexanone, 2-octanone, 4-hydroxy-4-methyl-2-pentanone and 1-methyl-2-pyrrolidone, as such or in admixture in an amount of 10 to 90% by
  • additives selected from the group of defoamers, thixotropic agents, leveling agents, deaerators and adhesion promoters can furthermore be added in an amount of from 0 to 5% by weight, based on the total amount.
  • compositions in which the individual components are optimally combined with one another and suitably mixed with one another have, as already described above, a Temperature of 20 0 C a viscosity in a range of 6 to 35 Pa - s and at the same time a shear rate of up to 25 s "1 , preferably it is in the range of 10 to 25 Pa * s at a shear rate of 25 s ' 1 and most preferably at 15 to 20 Pa * s at a shear rate of 25 s -1 .
  • the novel compositions are used in the form of etching pastes with thixotropic, non-Newtonian properties, oxidic, transparent, conductive layers during the manufacturing process of products for OLED displays, LC displays or for photovoltaics, semiconductor technology, high-power electronics, solar cells or photodiodes in a suitable manner to structure.
  • the paste is applied in a single step on the surface to be etched over the entire surface or according to the ⁇ tz Modellvorlage targeted only at the points on the surface or printed on where an etching is desired and after a predetermined exposure time after etching removed again by using a solvent or a solvent mixture is rinsed or the etching paste is burned by heating. After removal by heating, the treated surface can be rinsed off again, if necessary, for cleaning and removal of possibly remaining residues of the etching paste.
  • the etching paste composition is applied to the surface to be etched and removed again after an exposure time of 10 seconds to 15 minutes, preferably after 30 seconds to 2 minutes.
  • This approach is particularly suitable for the treatment of inorganic, glassy, crystalline surfaces as they must be formed and processed in processes of the semiconductor industry.
  • the surface to be etched may be a surface or partial surface of oxidic, transparent, conductive material, and / or a surface or partial surface of a porous and non-porous layer of oxide, transparent, conductive material on a carrier material.
  • the etching of the surfaces to be treated takes place at elevated temperatures in the range from 30 to 330 ° C., preferably in the range from 40 to 200 ° C., and very particularly preferably from 50 to 120 ° C.
  • doped tin oxide surfaces ITO and / or FTO
  • ITO and / or FTO doped tin oxide surfaces
  • the etching is carried out with etching rates of 1 to 6 nm / s, in particular with etching rates of 3 to 4 nm / s.
  • etching paste For the transfer of the etching paste to the substrate surface to be etched, a suitable method of printing technology with a high degree of automation and throughput is used.
  • a suitable method of printing technology with a high degree of automation and throughput is used.
  • etching process can take place with or without energy input, e.g. take place in the form of heat radiation (with IR emitters).
  • the actual etching process is then carried out by washing the surfaces with water and / or a suitable th solvent or mixture ended. Namely, after etching has taken place, the residues of the originally printable etching pastes with non-Newtonian flow behavior are rinsed off the etched surfaces with a suitable solvent or solvent mixture. The drying of the treated surfaces takes place in a known manner.
  • solvents may be added to the water, or other solvents may be used alone or in admixture.
  • solvents may be added to the water, as have already been used for the preparation of the compositions. Corresponding solvents are already mentioned above.
  • other solvents generally known to those skilled in the art for this purpose from the semiconductor art may be used.
  • Solvents having suitable physical properties may be used alone or in admixture. Solvents which have a good dissolving power for the paste residues on the surfaces and have a suitable vapor pressure are preferably used, so that after the surfaces have been rinsed, a problem-free drying is possible and, at the same time, has environmentally friendly properties.
  • the etching paste according to the invention has a viscosity in the range from 5 to 100 Pa s, preferably from 10 to 50 Pa s.
  • the viscosity is the substance-dependent proportion of the frictional resistance, which counteracts the movement when moving adjacent liquid layers.
  • the shear resistance in a fluid layer between two sliding surfaces arranged in parallel and moving relative to one another is proportional to the speed or shear gradient G.
  • the proportionality factor is a substance constant, which is called dynamic viscosity and has the dimension m Pa s.
  • the proportionality factor is pressure and temperature dependent. The degree of dependency is determined by the material composition. Inhomogenously composed liquids or substances have non-Newtonian or pseudoplastic properties. The viscosity of these substances is additionally dependent on the shear rate.
  • the more pronounced pseudoplastic or thixotropic properties of the etching paste compositions have a particularly advantageous effect on the screen or stencil printing and lead to significantly improved results.
  • this manifests itself in a shortened etching time, or with a constant etching time in an increased etching rate and above all in a larger etching depth with thicker layers.
  • iron (III) chloride, iron (III) chloride hexahydrate, and / or hydrochloric acid solutions at temperatures above 5O 0 C are capable of doped tin oxide surfaces (ITO) of 200 nm layer thickness within a few seconds Completely erase the minutes. At 100 ° C, the etching time is about 60 seconds.
  • the solvents, etching components, thickeners and additives are successively mixed with one another and stirred for a sufficient time until a viscous paste with thixotropic properties has formed.
  • the stirring can be carried out with heating to a suitable temperature. Usually, the components are stirred together at room temperature.
  • Preferred uses of the printable etching pastes according to the invention result for the described methods for structuring ITO applied to a carrier material (glass or silicon layer), for producing OLED displays, TFT displays or thin-film solar cells.
  • the pastes can be applied as already mentioned by means of dispenser technology.
  • the paste is filled in a plastic cartridge.
  • a dispenser needle is turned on the cartridge.
  • the cartridge is connected to the dispenser control via a compressed air hose.
  • the paste can then by compressed air through the
  • Dispenser needle are pressed.
  • the paste can be applied as a fine line to a substrate, for example an ITO-coated glass).
  • a substrate for example an ITO-coated glass.
  • different widths of paste lines can be generated.
  • Another possibility of the paste application is screen printing.
  • the etch pastes may be printed through a fine mesh screen containing the stencil sheet (or etched metal screens).
  • the pastes are burned in, whereby the electrical and mechanical properties can be determined.
  • baking firing through the dielectric layers
  • the applied etching pastes can be washed off after a certain exposure time with a suitable solvent or solvent mixture. The etching process is stopped by the washing.
  • an etching paste as described, for example, in Example 1, is produced.
  • a layer of doped tin oxide (ITO) of 120 nm thickness can be by screen printing within 60 seconds at 120 0 C selec- tively removed.
  • the etching is then terminated by immersing the Si wafer in water and then rinsing with the help of a finely divided water jet.
  • Atzpaste consisting of homogeneous thickening agent To a solvent mixture consisting of
  • Dispensing needle inside diameter 230 -260 ⁇ m

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • Weting (AREA)
  • Manufacturing Of Electric Cables (AREA)
  • Photovoltaic Devices (AREA)
  • Electroluminescent Light Sources (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

La présente invention concerne un nouvel agent dispersible destiné à la gravure de couches d'oxyde d'étain dopées ayant une viscosité non newtonienne pour graver les surfaces dans la production d'écrans et/ou de cellules solaires ainsi que leur utilisation. Il s'agit notamment de compositions exemptes de particules correspondantes qui permettent la gravure sélective de fines structures sans endommager ni attaquer les surfaces adjacentes.
EP06754211A 2005-07-04 2006-06-08 Agent de gravure de couches conductrices transparentes oxydantes Withdrawn EP1899277A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005031469A DE102005031469A1 (de) 2005-07-04 2005-07-04 Medium zur Ätzung von oxidischen, transparenten, leitfähigen Schichten
PCT/EP2006/005460 WO2007003255A1 (fr) 2005-07-04 2006-06-08 Agent de gravure de couches conductrices transparentes oxydantes

Publications (1)

Publication Number Publication Date
EP1899277A1 true EP1899277A1 (fr) 2008-03-19

Family

ID=36888644

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06754211A Withdrawn EP1899277A1 (fr) 2005-07-04 2006-06-08 Agent de gravure de couches conductrices transparentes oxydantes

Country Status (10)

Country Link
US (1) US20080210660A1 (fr)
EP (1) EP1899277A1 (fr)
JP (1) JP5373394B2 (fr)
KR (1) KR20080025757A (fr)
CN (1) CN101208277B (fr)
DE (1) DE102005031469A1 (fr)
HK (1) HK1119652A1 (fr)
MY (1) MY157618A (fr)
TW (1) TWI391474B (fr)
WO (1) WO2007003255A1 (fr)

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JP5373394B2 (ja) 2013-12-18
WO2007003255A1 (fr) 2007-01-11
JP2008547232A (ja) 2008-12-25
CN101208277B (zh) 2014-09-24
KR20080025757A (ko) 2008-03-21
CN101208277A (zh) 2008-06-25
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TWI391474B (zh) 2013-04-01
WO2007003255A8 (fr) 2007-03-22

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