Classifications

• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B23/00—Record carriers not specific to the method of recording or reproducing; Accessories, e.g. containers, specially adapted for co-operation with the recording or reproducing apparatus ; Intermediate mediums; Apparatus or processes specially adapted for their manufacture
  • G11B23/38—Visual features other than those contained in record tracks or represented by sprocket holes the visual signals being auxiliary signals
  • G11B23/40—Identifying or analogous means applied to or incorporated in the record carrier and not intended for visual display simultaneously with the playing-back of the record carrier, e.g. label, leader, photograph
• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
  • G11B7/252—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of layers other than recording layers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
  • B41J11/00—Devices or arrangements  of selective printing mechanisms, e.g. ink-jet printers or thermal printers, for supporting or handling copy material in sheet or web form
  • B41J11/0015—Devices or arrangements  of selective printing mechanisms, e.g. ink-jet printers or thermal printers, for supporting or handling copy material in sheet or web form for treating before, during or after printing or for uniform coating or laminating the copy material before or after printing
  • B41J11/002—Curing or drying the ink on the copy materials, e.g. by heating or irradiating
  • B41J11/0021—Curing or drying the ink on the copy materials, e.g. by heating or irradiating using irradiation
  • B41J11/00214—Curing or drying the ink on the copy materials, e.g. by heating or irradiating using irradiation using UV radiation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
  • B41J3/00—Typewriters or selective printing or marking mechanisms characterised by the purpose for which they are constructed
  • B41J3/407—Typewriters or selective printing or marking mechanisms characterised by the purpose for which they are constructed for marking on special material
  • B41J3/4071—Printing on disk-shaped media, e.g. CDs
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
  • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
  • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
  • B41M5/52—Macromolecular coatings
  • B41M5/5209—Coatings prepared by radiation-curing, e.g. using photopolymerisable compositions
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
  • B41M7/00—After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock
  • B41M7/0081—After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock using electromagnetic radiation or waves, e.g. ultraviolet radiation, electron beams
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
  • B41M2205/00—Printing methods or features related to printing methods; Location or type of the layers
  • B41M2205/12—Preparation of material for subsequent imaging, e.g. corona treatment, simultaneous coating, pre-treatments
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
  • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
  • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
  • B41M5/52—Macromolecular coatings
  • B41M5/5227—Macromolecular coatings characterised by organic non-macromolecular additives, e.g. UV-absorbers, plasticisers, surfactants
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
  • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
  • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
  • B41M5/52—Macromolecular coatings
  • B41M5/5254—Macromolecular coatings characterised by the use of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. vinyl polymers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
  • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
  • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
  • B41M5/52—Macromolecular coatings
  • B41M5/5263—Macromolecular coatings characterised by the use of polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • B41M5/5272—Polyesters; Polycarbonates
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
  • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
  • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
  • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
  • B41M5/52—Macromolecular coatings
  • B41M5/5263—Macromolecular coatings characterised by the use of polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • B41M5/5281—Polyurethanes or polyureas

Definitions

• the present invention relates to a method of printing on optical discs.
• Optical discs include compact discs (CDs) and digital versatile discs (DVDs) of various kinds including formats such as Blu-ray Disc and HD-DVD. They are designed to carry data (including audio or video information) which may be read by a laser or other optical device. Pre-recorded or replicated discs commonly have, on the side opposite that read by the laser or other optical device, a top layer of printing either to indicate the nature of the information on the disc or simply for decorative purposes. In the case of compact discs, for example, the area to be decorated is both the disc material, typically polycarbonate, and a spin coated layer used to protect the recording medium. It is desirable that this printing should be durable, water- and grease-resistant and inexpensive.
• UV energy curable, ink jet inks are known. These are normally free from water or organic solvents and "dry” by curing as a result of the polymerisation induced by exposure to UV (ultraviolet) or other radiation, e.g. electron beam. Unlike their water-based equivalents, once cured they can provide a hard, durable surface which is resistant to water, oils, bodily fluids and most domestically available fluids, and which is resistant to abrasion.
• UV ink jet inks suitable for use with high definition print heads such as XAAR Omnijet 318 do not print well onto conventional optical discs, either with or without a base coating of the types described above.
• the coating can often be removed by scratching, even with a fingernail, and the image printed is generally of poor quality, giving a "washed-out” or faded appearance due to poor printed dot formation. It should also be noted that best visual results are obtained when the jet printed image is backed-up with a solid colour and, in particular, white.
• the present invention consists in an optical disc having an optically readable side and a printed side, the printed side bearing a radiation-cured receptive coating formed by radiation curing a composition comprising a prepolymer, at least one monomer, and a levelling additive, said composition being free from any surface- modifying additives that would interfere with printability, and the cured composition being water-insoluble and non-absorbing to water.
• the cured coating should have a high degree of solvent resistance to promote wetting of the ink jet ink on the surface and to avoid softening and penetration of the ink jet composition into the coating layer.
• the invention provides an optical disc having, on an optically readable side and a printed side, the printed side bearing a radiation-cured receptive coating formed by radiation curing a composition comprising a prepolymer, at least one monomer, and a levelling additive, said composition being free from any silicone surface-modifying additives, and the cured composition being water-insoluble and non-absorbing to water.
• the receptive coating does not absorb the ink applied to it; instead, the ink sits on top of the coating and is cured by radiation, e.g. UV or electron beam.
• radiation e.g. UV or electron beam.
• the composition is to be cured by UV energy, it should include, in addition to the components mentioned above, a photoinitiator. Where it is to be cured by electron beam (EB), a photoinitiator is not necessary.
• the composition forming the receptive layer is free from silicone or similar surface modifying agents, a radiation-curable ink jet ink will adhere well to the surface of the cured composition.
• the cured receptive coating should also be water-insoluble and non-absorbing to water.
• the invention further provides a process in which a radiation-curable jet ink is jet printed onto a cured receptive coating, as defined above, on one side of an optical disc, and the ink is then cured by exposure to curing radiation.
• composition of the receptive coating may vary over a wide range. It should contain at least the following components:
• composition optionally and preferably contains either one or both of:
• the composition used to prepare the receptive coating advantageously comprises at least one prepolymer or combination of prepolymers.
• Suitable prepolymers include epoxy acrylates, acrylated oils, urethane acrylates, polyester acrylates, polyether acrylates, acrylated amines, acrylic saturated resins, acrylic acrylates, cycloaliphatic epoxides (cationic), phenol epoxy novolacs and acrylated epoxidised soya bean oils.
• the prepolymer has a number average molecular weight greater than 500 and more preferably greater than 800.
• the receptive coating preferably comprises no less than 10% and preferably no less than 20% by weight of one or more such prepolymers, based on the total weight of the composition.
• the receptive coating comprises not more than 50% and more preferably not more than 40% by weight of prepolymer based on the total weight of the composition.
• the prepolymer may be present in an amount if from 1% to 60% and preferably from 20% to 40% by weight based on the total weight of the composition.
• the prepolymer has a number average molecular weight of more than 500 and is present at a level of from 20% to 40% by weight based on the total weight of the composition.
• Preferred prepolymers exhibit a low level of shrinkage on curing.
• epoxy acrylates are preferred, bisphenol A epoxy acrylates and modified bisphenol A epoxy acrylates (modified, for example by the incorporation of amino, hydroxy, polyester and ethoxy groups during manufacture) being more preferred.
• the radiation-curable monomer is preferably an ethylenically unsaturated compound, for example an acrylate, a methacrylate or a vinyl compound, or a compound capable of polymerising by a ring-opening mechanism.
• Methacrylate monomers include the methacrylate equivalents of the acrylates described above, and notably hexanediol dimethacrylate, trimethylolpropane triacrylate, triethylene glycol dimethacrylate, diethylene glycol dimethacrylate, ethyleneglycol dimethacrylate, and 1 ,4-butanediol dimethacrylate.
• Non-acrylated reactive diluents that may be incorporated include vinyl components such as iV-vinylpyrrolidones, JV-vinylcaprolactams, JV-vinylformamide, vinyl ethers and styrenes.
• JV-Vinylcaprolactam (VCAP) has been found to be a particularly suitable vinyl monomer for inclusion in the compositions used to prepare the receptive coating of the invention due to its good adhesion to optical disc substrates.
• Vinyl ether compounds including ⁇ , ⁇ -unsaturated ether monomers such as triethylene glycol divinyl ether, diethylene glycol divinyl ether, 1 ,4-cyclohexanedimethanol divinyl ether and ethylene glycol mono vinyl ether, as well as ethyl 1 propenyl ether, triethylene glycol methyl propenyl ether, Methylene glycol methyl vinyl ether and 2-cyclopenten- 1-yl ether may also be used.
• Other monomers include acryloyl morpholine.
• Suitable oxygen-containing ring opening monomers include those comprising an oxetane ring or an oxirane ring.
• Oxirane species include cycloaliphatic oxiranes (also known as epoxides), such as 3,4-epoxy cyclohexyl methyl-3,4-epoxy cyclohexyl carboxylate and the glycidyl ethers of polyols.
• Oxiranes derived by the epoxidation of unsaturated materials may also be suitable, for example, epoxidised soybean oil, epoxidised polybutadiene or epoxidised alkenes.
• Oxetane species include mono- functional and multi-functional oxetanes, for example, 3-ethyl-3-hydroxymethyl- oxetane, bis[(l-ethyl-3-oxetanyl)methyl] ether, 3-ethyl-3-[2- ethylhexyloxy)methyl]oxetane, [ 1 ,4-bis(3 -ethyl-3 -oxetanylmethoxy)methyl]benzene and trimethylolpropane oxetane. Many further suitable materials are known to the skilled person.
• the prepolymer and the monomer(s) should be selected for high surface tension, so that the composition has a surface tension higher than that of the ink jet ink which is to be printed onto it.
• the prepolymer preferably has a surface tension of at least 35 mN per m (dynes per cm 2 ), more preferably at least 38 mN per m (dynes per cm 2 ), whilst the monomer(s) should preferably have a surface tension of at least 32 mN per m (dynes per cm 2 ), more preferably at least 35 mN per m (dynes per cm 2 ).
• the receptive coating may be free-radically curable, cationically curable or it may be curable by a combination of the two mechanisms. It may also be curable by electron beam. If the coating is to be cured by UV energy, then a photoinitiator may be necessary. The nature of the photoinitiator used will depend on the curing mechanism desired, but is otherwise not critical to the present invention.
• the photoinitiators may be of the cleavage or hydrogen abstraction type and are preferably selected from the following photoinitiator classes: benzophenones, thioxanthones and related compounds, hydroxyalkylphenones, aminoalkylphenones, anthraquinones, standard and modified acyl phosphine oxides (such as Lucirin TPO and TPO-L), bis-acyl phosphine oxides (such as Irgacure 819), benzil ketals, benzoin ethers, acetophenones, beta ketosulphones, oxime esters and phenyl glyoxic acid esters.
• benzophenones thioxanthones and related compounds
• hydroxyalkylphenones aminoalkylphenones
• anthraquinones anthraquinones
• standard and modified acyl phosphine oxides such as Lucirin TPO and TPO-L
• cationic photoinitiators include sulphonium salts (such as the mixture of compounds available under the trade name UVI6992 from Dow Chemical), thianthrenium salts (such as Esacure 1187 available from Lamberti), iodonium salts (such as IGM 440 from IGM), phenacyl sulphonium salts, and the thioxanthonium salts, such as those described in WO 03/072567 Al, WO 03/072568 Al, and WO 2004/055000 Al, the disclosures of which are incorporated herein by reference , such as those sold under the trade marks IGM 550 and IGM 650 by IGM.
• sulphonium salts such as the mixture of compounds available under the trade name UVI6992 from Dow Chemical
• thianthrenium salts such as Esacure 1187 available from Lamberti
• iodonium salts such as IGM 440 from IGM
• phenacyl sulphonium salts such as those described in WO 03
• the photoinitiator used is preferably one which does not require the additional use of an amine synergist, and, in particular, it is preferred that the composition should not include a non-acrylated free amine synergist.
• the receptive coating is to be white, it is generally preferred that the photoinitiator should be non-yellowing. Where, however, it is to be another colour, this is unnecessary.
• the receptive coating should be such that the receptive coating wets the optical disc substrate sufficiently well to form a film on the substrate when applied by screen printing.
• the receptive coating adheres well to the disc material or spin coat, enabling the receptive coating to adhere well to the disc, without swelling or otherwise distorting the disc material, thereby promoting good adhesion.
• composition of the present invention also contains surface active agents to improve, for example, levelling, wetting and defoaming properties.
• surface active materials should have a low tendency to migrate to the coating surface and thereby adversely affect its receptivity.
• Suitable materials are silicone free and may be polymeric in nature. Examples of such compounds include polymeric acrylates, mineral oil blends, low temperature wax dispersions and paraffinic wax dispersions, for example Modafiow TM (Cytec), BYK A501 (BYK), Bevaloid 6681 (Rhone Poulenc), BYK 1790, BYK A500, BYK A560, Tego Airex 910 and Tego Airex 920.
• fluorosurfactant may be added to the composition to improve surface wetting during application.
• fluorosurfactants include Zonyl FSNlOO, Zonyl FSOlOO ex Dupont and Fluorad 4430 ex 3M.
• the composition used to prepare the receptive coating the present invention may optionally contain a pigment or other colorant, preferably a pigment.
• a pigment or other colorant preferably a pigment.
• the term 'colorant' covers materials which endow an actual visual colour, which may be, and preferably is, white.
• White pigments are typically included in amounts of about 40-50% by weight of the total composition.
• the actual amount of colorant used may vary widely depending on the nature of the colorant, for example within the range of from 1 to 60% by weight, more preferably from 7 to 50% by weight. If it is desired that the coating should be clear, then no colorant need be included.
• colorants may be considered as falling into two classes, namely dyes, which are substantially soluble in the ink composition, and pigments, which are dispersed in the ink composition in the form of fine particles, if necessary with the aid of a suitable dispersant.
• Pigments may be selected from a wide range of classes, for example, Pigment Red 146, Pigment Red 170, Pigment Red 48:2, Pigment Red 122, Pigment Blue 15:3, Pigment Violet 23, Pigment Green 7, Pigment Yellow 83, Pigment Yellow 13, Pigment Yellow 17, Pigment Black 7.
• suitable pigments are given in "Printing Ink Manual", fourth edition, Leach R. H. et al.
• the pigment if used, is preferably a white pigment, for example Pigment White 6 titanium dioxide e.g. Kemera RDI-S, Rronos 1070, Kronos 1071, Tipure R706 or zinc oxide, zinc sulphide or barium sulphate, of which titanium dioxide is preferred.
• Pigment White 6 titanium dioxide e.g. Kemera RDI-S, Rronos 1070, Kronos 1071, Tipure R706 or zinc oxide, zinc sulphide or barium sulphate, of which titanium dioxide is preferred.
• a combination of any two or more of these colorants may be used, if desired, in order to achieve particular effects.
• formulations may also contain extenders and fillers in order to further improve the behaviour and appearance of the ink both during and after print processing.
• Typical generic examples of preferred fillers and extenders are synthetic and natural grades of chalk, talc, kaolin and other aluminium hydroxides and silicates. They are known commercially under many trade names, examples of which are Calcigloss, Microtalc, Speswhite, Spacerite and Zeolex.
• formulations may also be modified with small amounts of a structuring additive, such as fumed silica or activated bentonite, in order to produce the preferred rheo logical behaviour on the screen printing presses.
• a structuring additive such as fumed silica or activated bentonite
• examples of such materials are Aerosil from Degussa, Bentone SDl, Bentone SD2, Bentone 34 ex Elementis and Tixogel DS, Tixogel VPA, Tixogel MPlOO from Sud Chemie.
• composition of the present invention may be present in a wide range of quantities, depending on the desired physical and chemical properties of the final cured coating.
• compositions of the present invention may be prepared by simple mixing and dispersion techniques as are well known in the art, and may be applied to the optical disc by any well known printing technique, e.g. screen printing, spin coating, pad printing or flexographic printing, preferably screen printing.
• printing technique e.g. screen printing, spin coating, pad printing or flexographic printing, preferably screen printing.
• the whole of one surface of the optical disc may be coated, or only a portion may be coated.
• the coating may then be cured, using any well known technique of radiation curing.
• the invention is further illustrated by the following non-limiting Examples.
• the following screen ink composition was prepared by first premixing the materials and then grinding the resultant mixture on a triple roll mill until a grind of ⁇ 12 microns ( ⁇ m) was achieved.
• Titanium Dioxide White Pigment anatase 49.1
• the resulting screen ink composition was printed through a 150-31 mesh onto an optical media substrate (CDR, DVD-R) and cured using a medium pressure mercury lamp (80WCm "1 ).
• a 4 colour high definition test image was ink jet printed on top of the cured coating using a commercial UV ink jet ink through a XAAR Omnijet 318 piezo DOD print head and UV cured.
• the resultant prints were examined for image quality and durability. The results are shown in the following Table 1.
• the following screen ink composition was prepared by first premixing the materials and then grinding the resultant mixture on a triple roll mill until a grind of ⁇ 12 microns ( ⁇ m) was achieved.
• the resulting screen ink composition was printed through a 150-31 mesh onto an optical media substrate (CDR, DVD-R) and cured using a medium pressure mercury lamp (80WCm "1 ).
• a 4 colour high definition test image was ink jet printed on top of the cured coating using a commercial UV ink jet ink through a XAAR Omnijet 318 piezo DOD print head and UV cured.
• the resultant prints were examined for image quality and durability. The results are shown in the following Table 1.
• the following screen ink composition was prepared by first premixing the materials and then grinding the resultant mixture on a triple roll mill until a grind of ⁇ 12 microns ( ⁇ m) was achieved.
• the resulting screen ink composition was printed through a 150-31 mesh onto an optical media substrate (CDR, DVD-R) and cured using a medium pressure mercury lamp (80Wcm-l).
• a 4 colour high definition test image was ink jet printed on top of the cured coating using a commercial UV ink jet ink through a XAAR Omnijet 318 piezo DOD print head and UV cured.
• the resultant prints were examined for image quality and durability. The results are shown in the following Table 1.
• This Example uses a silicone antifoaming agent in place of the silicone-free levelling agent of the present invention.
• the following screen ink composition was prepared by first premixing the materials and then grinding the resultant mixture on a triple roll mill until a grind of ⁇ 12 microns ( ⁇ m) was achieved.
• the resulting screen ink composition was printed through a 150-31 mesh onto an optical media substrate (CDR, DVD-R) and cured using a medium pressure mercury lamp (80Wcm-l).
• a 4 colour high definition test image was ink jet printed on top of the cured coating using a commercial UV ink jet ink through a XAAR Omnijet 318 piezo DOD print head and UV cured.
• the resultant prints were examined for image quality and durability. The results are shown in the following Table 1.
• the following screen ink composition was prepared by first premixing the materials and then grinding the resultant mixture on a triple roll mill until a grind of ⁇ 12 microns ( ⁇ m) was achieved.
• the resulting screen ink composition was printed through a 150-31 mesh onto an optical media substrate (CDR, DVD-R) and cured using a medium pressure mercury lamp (80Wcm-l).
• a 4 colour high definition test image was ink jet printed on top of the cured coating using a commercial UV ink jet ink through a XAAR Omnijet 318 piezo DOD print head and UV cured.
• the resultant prints were examined for image quality and durability. The results are shown in the following Table 1.

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• Health & Medical Sciences (AREA)
• General Health & Medical Sciences (AREA)
• Toxicology (AREA)
• Physics & Mathematics (AREA)
• Electromagnetism (AREA)
• Optical Record Carriers And Manufacture Thereof (AREA)
• Ink Jet Recording Methods And Recording Media Thereof (AREA)
• Ink Jet (AREA)
• Inks, Pencil-Leads, Or Crayons (AREA)
• Manufacturing Optical Record Carriers (AREA)

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• 2006
  • 2006-05-05 GB GB0608948A patent/GB2437714A/en not_active Withdrawn
• 2007
  • 2007-05-03 JP JP2009510069A patent/JP2009536425A/ja active Pending
  • 2007-05-03 WO PCT/US2007/068122 patent/WO2007131098A2/en not_active Ceased
  • 2007-05-03 EP EP07761808A patent/EP2024973A2/de not_active Withdrawn
  • 2007-05-03 CN CNA2007800254237A patent/CN101484946A/zh active Pending

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