EP1758713B1 - Materiau abrasif et procede de formation associe - Google Patents
Materiau abrasif et procede de formation associe Download PDFInfo
- Publication number
- EP1758713B1 EP1758713B1 EP05754973A EP05754973A EP1758713B1 EP 1758713 B1 EP1758713 B1 EP 1758713B1 EP 05754973 A EP05754973 A EP 05754973A EP 05754973 A EP05754973 A EP 05754973A EP 1758713 B1 EP1758713 B1 EP 1758713B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- protrusions
- base
- abrasive material
- photoresist
- butte
- 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
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D11/00—Constructional features of flexible abrasive materials; Special features in the manufacture of such materials
Definitions
- the present invention relates to an abrasive material suitable for sanding or smoothing a variety of surfaces.
- abrading surfaces have been suggested over the years. Such surfaces include those wherein abrasive particles such as garnet, aluminum oxide, silicon carbide, grit of zirconia and alpha aluminum oxide monohydrate, single crystals of diamond or cubic boron nitride are adhered to a substrate. Also known are abrasive surfaces which are scored to provide grooves or punched to provide holes or openings with projections or burs surrounding the holes. Where grooves have been formed in metal sheets such as steel sheets, coating the surface or the cutting edge formed by the groove are also known. Metal abrasive sheets are known which are prepared by forming a cured polyvinylchloride negative master using a sheet of sandpaper and, then, electroplating the master to form the sheet.
- abrasive particles such as garnet, aluminum oxide, silicon carbide, grit of zirconia and alpha aluminum oxide monohydrate, single crystals of diamond or cubic boron nitride are adhered to a substrate.
- Etching processes using a suitable resist to form a desired pattern in a metal substrate are also known.
- a resist pattern is applied to a thin flat steel plate in a predetermined pattern such as equal sized spots which can be round, elongate or polygonal.
- the plate is etched which an etchant such as an aqueous solution of ferric chloride to remove the desired amount of metal and form the pattern elements.
- an etchant such as an aqueous solution of ferric chloride
- the cutting teeth are formed in the shape of triangles or squares which come out of the etch process still sharp and usable due to the resist pattern which accentuates the corner points and eliminates under cutting of the upper surfaces of the cutting teeth.
- Each tooth bears an upper flat surface and is amenable to hardening by heat treating without excessive brittleness due to the tooth configuration.
- the upper flat surface of each tooth is reported to be typically about 3 mils with the width of the base and the height of the tooth being about twice that of the upper flat surface.
- a process for producing cutting dies, particularly for use such as, for example, cutting adhesive tape to form labels, has been disclosed wherein multiple etching steps are used.
- a resist corresponding to the contour of a label to be propertied is formed on a steel plate and a first etching step is carried out, thereby forming a convex portion of a prescribed height.
- a second etching step is carried out whereby the resist extending from both sides of the top of[f] the convex portion is removed and the steel plate is subjected to further etching. This second etching step may be carried out multiple times. The resist remaining on the top of the convex portion is then removed.
- a metal abrasive has been described having substantially uniform pyramidal protrusions extending from a base surface which is formed by etching of metal sheet material.
- An abrasive material according to the preamble of claim 1 is known from WO-A-97/06 928 , for example.
- the present invention provides an abrasive material comprising a base surface having a plurality of pyramidal shapes and a plurality of butte-like shapes protruding therefrom, the base surface and the protrusions being formed of the same material, a portion of the protrusions having a substantially triangular, square, or polygonal base and triangular sides which meet at an apex which substantially forms a point, hereinafter pyramids, and a portion of the protrusions having a substantially triangular, square, or polygonal base and substantially trapezoidal sides, the portions sides distant from the base surface forming a plateau such that the protrusions are substantially butte-like in shape, hereinafter termed buttes, the protrusions providing intermixing cutting and planing edges in a pattern such that the material is capable of abrading independent of direction of use.
- the ratio of the pyramids to the buttes is preferably about 90:10 to 10:90, more preferably about 75:25 to 25:75, most preferably about 50:50 to 25:75.
- the ratio of pyramids to buttes is preferably such that the plateaus of the buttes serve as a gliding surface for the abrasive material. This combination of buttes and pyramids provides the abrasive material with the capability to refine and smooth a surface being abraded without excessive removal of surface material.
- the pyramids of an abrasive material of the invention may be the same or different in shape.
- various pyramidal shapes may have different bases configurations, i.e., different numbers of sides, and/or different degrees of slope.
- the buttes of an abrasive material of the invention may be the same or different in shape.
- Optional performance enhancing surface treatments may be applied to the protrusions and/or the base surface to improve abrasive performance, aid in non-loading characteristics due to the lubricity of certain coatings, and reduce surface porosity.
- the triangular sides of the pyramids and the trapezoidal sides of the buttes have an inward arcuate slope. Such slopes provide greater longevity of the abrasive material due to lack of loading of material being abraded.
- the present invention provides rapid material removal from a workpiece, yet leaves a smooth surface on the workpiece.
- the abrasive material of the invention can be provided with protrusions on both surfaces of the base material to prevent curling when the material is thin.
- protrusions can be provided on one surface and the opposing surface can simply be etched.
- the surface of the protrusions and the base surface can optionally be provided with performance enhancing coatings or treatments to improve abrasive performance, aid in non-loading characteristics due to the lubricity of certain coatings, and reduce surface porosity.
- Plating can be used to provide such enhanced surfaces.
- the surface can be heat treated or metallurically altered to form a thin harder layer on the surface of the base surface and protrusions to improve hardness as is well known to those skilled in the art.
- Other performance enhancing treatments such as, for example, diamond surface treatments can be useful. A particularly useful diamond surface treatment using laser technology is described in U.S. Patent No. 5,620,754 .
- FIGS. 1A, 1B, and 1C are perspective views of pyramidal protrusions useful in the invention.
- FIG. 2 is a perspective view of a preferred pyramidal protrusion of the invention having inward arcuate triangular sides which meet at an apex which substantially forms a point.
- FIG. 3 is a perspective view of a preferred butte protrusion of the invention having inward arcuate triangular sides and a plateau distant from the base surface.
- FIG. 4A is a top view of a photoresist mask suitable for use in producing an abrasive material of the invention.
- FIG. 4B is a top view of another photoresist mask suitable for use in producing an abrasive material of the invention.
- FIG.4C is a top view of another photoresist mask suitable for use in producing an abrasive material of the invention.
- FIG. 4D is a top view of another photoresist mask suitable for use in producing an abrasive material of the invention.
- FIG. 5 is side view of a pyramidal protrusion useful in the invention having a performance enhancing coating thereon.
- FIG. 6 is a fragmented cross-section of an abrasive material of the present invention having pyramidal protrusions on each surface thereof.
- the abrasive material of the invention can be formed from any material susceptible to etching including, for example, stainless steel, carbon steel, aluminum alloys, iron-nickel-chrome alloys, and titanium; boron-filled elastomers, silica composites, fluorocarbon materials, graphite alloys, plastics, and the like.
- Stainless steel is a particularly preferred base material in the present invention due to the intrinsic resistance of the material to corrosion, the good high and excellent low temperature strength and toughness over a broad range of temperatures, the non-magnetic properties of austenitic grades, and aesthetic appeal. Stainless steel can also be readily reproducibly etched to form the abrasive material of the invention.
- the thickness of the material is not particularly limited, but after etching should be suitably flexible where it will be used over a roller or suitably stiff when used as a flat abrasive.
- stiffness can be provided, if necessary, by attachment to a stiff substrate such as, for example, a metal plate or synthetic resin plate having suitable stiffness.
- Typical surface treatments particularly preferred for stainless steel base material include, but are not limited to, nickel or chrome plating or diamond coating or plating in combination with diamond dust or boron nitride.
- the base and pyramidal protrusions can be exposed to heat treatment or metallurical alteration, e.g., case hardening, to effect, for example, surface hardness by forming a thin harder layer on the base surface and protrusions to improve performance.
- FIGS. 1A, 1B, and 1C depict various possible embodiments of the pyramidal protrusions of the abrading material of the invention with the bases of the pyramidal protrusions being triangular, square and pentagonal, respectively. Of course, other polygonal shapes can be used.
- protrusion 10a is shown having triangular base 12a, triangular side 14a, and apex 16a.
- protrusion 10b is shown having square base 12b, triangular side 14b and apex 16 b.
- protrusion 10c is shown having polygonal base 12c, triangular side 14c and apex 16c.
- the depth of the inward arcuate slope on the triangular sides of the protrusions can be from very slight, e.g., 1 ⁇ m, to as great as about 175 ⁇ m.
- Such arcuate slopes can readily be seen in FIG. 2 wherein pyramid 20 has arcuate sloped surfaces 24a meeting at apex 26 and in FIG. 3 wherein butte 21 has arcuate sloped surfaces 24d meeting at plateau 28.
- the height H of the pyramids and buttes from the etched surface can be in the range of about 25 ⁇ m to 1.5 mm, with higher protrusions for normal coarse abrading, i.e., from about 125 ⁇ m to 375 ⁇ m, and lower pyramidal protrusions for finer abrading, i.e., from about 75 ⁇ m to 125 ⁇ m.
- the length of the edges L of the base is dependent on the height of the protrusions.
- the ratio of the height of the protrusions from the etched surface to the length of the edge of the base is in the range of about 1:1 to 1:5, more preferably about 1:2 to 1:4, most preferably about 1:3.
- the thickness of the remaining base material B can vary widely and is not critical, with thinner base materials being used for more flexible abrasive materials and thicker base materials being used for stiffer abrasive materials as is well known to those skilled in the art. Such dimensions are indicated in the view of a pyramid of an abrasive material of the invention, seen in cross-section in FIG. 5 .
- the spacing S of the pyramids and buttes can also vary widely, from about 0.75 mm to 30 mm apart, as measured from center to center of the pyramidal protrusions in , with greater spacing for coarse abrading, i.e., 2 to 10 mm or more apart and less spacing for finer abrading, i.e., from about 0.75 to 1.5 mm apart.
- the fineness or coarseness of the abrasive material can also be adjusted by maintaining the height of the protrusions and the length of the base of the protrusions and adjusting the size of the resist pattern. Greater spacing between the protrusions provides coarser abrading material, while lesser spacing between the protrusions provides finer abrading material.
- FIG. 4A A portion of a photoresist mask suitable for a fine abrasive grit is shown in FIG. 4A .
- the pyramidal protrusions be oriented such that the cutting edges of the individual protrusions are oriented in different directions to provide the capability of abrading independent of direction of use.
- the pyramidal protrusions can be randomly oriented in various directions such as by designing the etching mask through the use of a computer-based random generator or an etching mask can be patterned which ensures random orientation as is well known to those skilled in the art. Examples of randomly oriented patterns are shown in the photoresist masks in FIGS. 4A , 4B , 4C and 4D .
- a coating such as nickel or chrome plating; a diamond coating; or nickel or chrome plating in combination with diamond dust or Teflon ® , tungsten, carbide or boron nitride particles can be applied to the surface of the abrasive material such as is shown in FIG. 5 , wherein a portion of abrasive material 59 has protrusion 52, remaining base material 54, and coating 56.
- the etching process can be carried out using well-known resist and etching materials and processes.
- cleaning of the base material Prior to application of the photoresist to the base material, cleaning of the base material is preferably carried out.
- the base material is stainless steel
- cleaning may involve rinsing with deionized water and drying.
- the stainless steel surface may also be subjected to a pumice scrub or passivation treatment. Passivation which removers free iron contaminants, if present, as well as other contaminants is generally carried out with the use of solutions of ferric chloride, nitric acid or other solutions know to those skilled in the art.
- the resist coating can be applied using, for example, hot roll lamination, screen printing, gravure printing, dip coating and the like.
- a resist is applied, in the form of a polymeric film to a stainless steel base material, the base material is preferably pre-heated and the film is applied using sufficient heat and pressure to ensure good adhesion. Curing of the resist must be avoided at this point in the process.
- the mask which is used to provide the desired abrasive pattern surface is then placed on the resist covered base material.
- Good, i.e., intimate, contact between the resist coating and the mask is needed to achieve the desired pattern on the base material when the photoresist not covered by the mask is cured. Such contact can be enhanced by use of vacuum techniques.
- Curing is achieved by exposure to light sufficient to cure, i.e., cross-link, the polymeric resist.
- the mask is then removed from the base material/photoresist/ mask composite and the uncured photoresist is removed from the base material using a developing solution, or developer.
- the selection of the developer is dependent on the composition of the photoresist. If desired, the photoresist then remaining on the base material may be imaged again prior to etching to further ensure good adhesion of the photoresist to the base material during etching.
- Etching is then performed on those portions of the base material not protected by the photoresist.
- suitable etchants include ferric chloride, hydrochloric acid, hydrofluoric acid, nitric acid, mixtures of these acids and sodium hydroxide; for aluminum or aluminum alloys, suitable etchants include sodium hydroxide; for titanium, suitable etchants include hydrofluoric acid; and plastics are generally etchable using various acids. The degree of etching can be adjusted by altering the concentration and temperature of the etchant solution and the method of application as is known to those skilled in the art.
- aqueous ferric chloride solution of about 37° to 42° Baume can be used, the lower the Baume of the solution, generally the more arcuate the slope of the sides of the protrusions.
- any remaining photoresist may optionally be removed by techniques well known to those skilled in the art. In some cases with certain mask patterns and etching parameters, much of the photoresist is removed in the etching process. Removal of remaining photoresist is generally preferable, particularly when the pyramidal protrusions are to be plated and the photoresist may act as a plating resist.
- the resist can be retained on the surface of the resultant abrasive material, particularly on the non-abrasive side of the material when only one side is masked and pattern etched, which aids in prevention of curling.
- a suitable method of preventing curling involves etching both surfaces of the base material as shown in FIG. 6 , wherein abrasive material 60 has protrusions 62a, 62b on each surface 61, 63 extending from the remaining base material 64.
- the stainless steel/photoresist/mask composite was exposed to 60 millijoules of light to effect initial imaging of the photoresist.
- the uncrosslinked photoresist was removed by rinsing with a developer solution of 1 % aqueous potassium carbonate at pH 10.5.
- the stainless steel having the photoresist pattern thereon was re-exposed to 100 millijoules light to ensure adherence of the photoresist to the stainless steel during etching.
- the stainless steel was etched to a depth of about 0.003 inches using a 40° Baume ferric chloride solution over a period of about 4 minutes.
- the resulting etched sheet was rinsed with water and remaining photoresist was removed using a 15% potassium hydroxide aqueous stripping solution.
- Pyramidal protrusions and butte protrusions having a triangular bases were formed.
- the height of the protrusions was about 0.003 inches. This resulting abrasive material equivalent to a medium grade sandpaper is suitable for finish sanding of drywall after taping and patching.
- the composite was etched using a 40 Baume ferric chloride solution for a time sufficient to etch to a depth of about 0.01 inch.
- An abrasive material having pyramids and buttes was formed which was equivalent in abrasiveness to a coarse grade sandpaper.
- a photoresist was applied as in Example 1.
- a mask having a pattern as shown in FIG[S]. 4A was applied over the photoresist as in Example 1.
- the composite was etched using a 40° Baume ferric chloride solution for a time sufficient to etch to a depth of about 0.0035 ⁇ 0.0005 inch.
- a sheet of 301 full hard stainless steel having a gauge of about 0.013 was cleaned using a pumice scrub and passivated for 30 seconds with an acid solution of ferric chloride.
- the stainless steel/photoresist/mask composite was crosslinked, rinsed, and re-exposed as in Example 1.
- the stainless steel was etched to a depth of about 0.008 inches using a 40° Baume ferric chloride solution over a period of about 6 minutes.
- the resulting etched sheet was rinsed with water and remaining photoresist was removed using a 15% potassium hydroxide aqueous stripping solution.
- Pyramidal protrusions and butte protrusions having a triangular bases were formed.
- the height of the protrusions was about 0.007 inches. This resulting abrasive material equivalent to a medium grade sandpaper is suitable for finish sanding of drywall after taping and patching.
- a sheet of 304 full hard stainless steel having a gauge of 0.010 was cleaned using a pumice scrub and passivated as in Example 1.
- a photoresist was applied, and developed as in Example 1 using a mask having a pattern as shown in FIG. 4A .
- the composite was etched using a 40° Baume ferric chloride solution to a depth of about 0.005 inch.
- An abrasive material having pyramids and buttes was formed which was equivalent in abrasiveness to a fine grade sandpaper, particularly suitable for finish sanding.
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Polishing Bodies And Polishing Tools (AREA)
- ing And Chemical Polishing (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Claims (1)
- Matériau abrasif comprenant une surface de base ayant une pluralité de formes pyramidales et une pluralité de formes de type butte saillant depuis celle-ci, une portion des saillies ayant une base substantiellement triangulaire, carrée ou polygonale et des côtés triangulaires qui se rejoignent au niveau d'un sommet qui forme substantiellement une pointe, et une portion des saillies ayant une base substantiellement triangulaire, carrée ou polygonale, et des côtés substantiellement trapézoïdaux, les côtés des portions espacés de la surface de base formant un plateau, de telle sorte que les saillies aient substantiellement une forme de butte, caractérisé en ce que les saillies fournissent des alternances de bords de coupe et de planage suivant un motif tel que ledit matériau soit en mesure d'effectuer une abrasion indépendamment du sens de l'utilisation, et les saillies de type butte fournissent aussi une surface substantiellement glissante, et en ce que la surface de base et les saillies sont formées du même matériau.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US84851004A | 2004-05-17 | 2004-05-17 | |
PCT/US2005/017997 WO2005112601A2 (fr) | 2004-05-17 | 2005-05-17 | Materiau abrasif et procede de formation associe |
Publications (3)
Publication Number | Publication Date |
---|---|
EP1758713A2 EP1758713A2 (fr) | 2007-03-07 |
EP1758713A4 EP1758713A4 (fr) | 2007-10-10 |
EP1758713B1 true EP1758713B1 (fr) | 2009-04-01 |
Family
ID=35428761
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP05754973A Not-in-force EP1758713B1 (fr) | 2004-05-17 | 2005-05-17 | Materiau abrasif et procede de formation associe |
Country Status (7)
Country | Link |
---|---|
EP (1) | EP1758713B1 (fr) |
JP (1) | JP2007537891A (fr) |
CN (1) | CN100577363C (fr) |
AT (1) | ATE427189T1 (fr) |
CA (1) | CA2566888A1 (fr) |
DE (1) | DE602005013666D1 (fr) |
WO (1) | WO2005112601A2 (fr) |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8142531B2 (en) * | 2008-12-17 | 2012-03-27 | 3M Innovative Properties Company | Shaped abrasive particles with a sloping sidewall |
US8480772B2 (en) | 2009-12-22 | 2013-07-09 | 3M Innovative Properties Company | Transfer assisted screen printing method of making shaped abrasive particles and the resulting shaped abrasive particles |
WO2013102177A1 (fr) | 2011-12-30 | 2013-07-04 | Saint-Gobain Ceramics & Plastics, Inc. | Particule abrasive façonnée et procédé de formation de celle-ci |
EP3705177A1 (fr) * | 2012-01-10 | 2020-09-09 | Saint-Gobain Ceramics & Plastics Inc. | Particules abrasives dotées de formes complexes et méthodes pour former les mêmes |
KR101736085B1 (ko) | 2012-10-15 | 2017-05-16 | 생-고뱅 어브레이시브즈, 인코포레이티드 | 특정한 형태들을 가진 연마 입자들 및 이러한 입자들을 형성하는 방법들 |
EP2978566B1 (fr) | 2013-03-29 | 2024-04-24 | Saint-Gobain Abrasives, Inc. | Particules abrasives ayant des formes particulières et procédés de formation de telles particules |
US9771507B2 (en) | 2014-01-31 | 2017-09-26 | Saint-Gobain Ceramics & Plastics, Inc. | Shaped abrasive particle including dopant material and method of forming same |
MX2016013465A (es) | 2014-04-14 | 2017-02-15 | Saint-Gobain Ceram & Plastics Inc | Articulo abrasivo que incluye particulas abrasivas conformadas. |
US9914864B2 (en) | 2014-12-23 | 2018-03-13 | Saint-Gobain Ceramics & Plastics, Inc. | Shaped abrasive particles and method of forming same |
US10196551B2 (en) | 2015-03-31 | 2019-02-05 | Saint-Gobain Abrasives, Inc. | Fixed abrasive articles and methods of forming same |
TWI634200B (zh) | 2015-03-31 | 2018-09-01 | 聖高拜磨料有限公司 | 固定磨料物品及其形成方法 |
CA2988012C (fr) | 2015-06-11 | 2021-06-29 | Saint-Gobain Ceramics & Plastics, Inc. | Article abrasif comprenant des particules abrasives profilees |
SI3455321T1 (sl) | 2016-05-10 | 2022-10-28 | Saint-Gobain Ceramics & Plastics, Inc. | Metode oblikovanja abrazivnih delcev |
KR102313436B1 (ko) | 2016-05-10 | 2021-10-19 | 생-고뱅 세라믹스 앤드 플라스틱스, 인코포레이티드 | 연마 입자들 및 그 형성 방법 |
US11230653B2 (en) | 2016-09-29 | 2022-01-25 | Saint-Gobain Abrasives, Inc. | Fixed abrasive articles and methods of forming same |
US10563105B2 (en) | 2017-01-31 | 2020-02-18 | Saint-Gobain Ceramics & Plastics, Inc. | Abrasive article including shaped abrasive particles |
WO2021133901A1 (fr) * | 2019-12-27 | 2021-07-01 | Saint-Gobain Ceramics & Plastics, Inc. | Articles abrasifs et leurs procédés de formation |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6080567A (ja) * | 1983-10-07 | 1985-05-08 | Mitsui Mining & Smelting Co Ltd | セグメント形固定砥粒研摩体の製造方法 |
SE464394B (sv) * | 1987-05-15 | 1991-04-22 | Sandvik Ab | Etsad verktygsplaat foer ytbearbetning samt metod foer framstaellning daerav |
US5366523A (en) * | 1992-07-23 | 1994-11-22 | Minnesota Mining And Manufacturing Company | Abrasive article containing shaped abrasive particles |
EP0846041B1 (fr) * | 1995-08-11 | 2003-04-23 | Minnesota Mining And Manufacturing Company | Procede de fabrication d'un article abrasif a revetement dote de multiples proprietes abrasives |
KR20010020307A (ko) * | 1998-02-27 | 2001-03-15 | 앤써니 폴라스키 | 연마재 및 그 제조 방법 |
JP3025884B1 (ja) * | 1998-11-20 | 2000-03-27 | 帝国クロム株式会社 | 帯板ヤスリの製造方法 |
US6821189B1 (en) * | 2000-10-13 | 2004-11-23 | 3M Innovative Properties Company | Abrasive article comprising a structured diamond-like carbon coating and method of using same to mechanically treat a substrate |
JP2003053665A (ja) * | 2001-08-10 | 2003-02-26 | Mitsubishi Materials Corp | ドレッサー |
-
2005
- 2005-05-17 DE DE602005013666T patent/DE602005013666D1/de active Active
- 2005-05-17 WO PCT/US2005/017997 patent/WO2005112601A2/fr active Application Filing
- 2005-05-17 EP EP05754973A patent/EP1758713B1/fr not_active Not-in-force
- 2005-05-17 JP JP2007527540A patent/JP2007537891A/ja active Pending
- 2005-05-17 CA CA002566888A patent/CA2566888A1/fr not_active Abandoned
- 2005-05-17 CN CN200580023977A patent/CN100577363C/zh not_active Expired - Fee Related
- 2005-05-17 AT AT05754973T patent/ATE427189T1/de not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
CN100577363C (zh) | 2010-01-06 |
WO2005112601A3 (fr) | 2006-07-06 |
ATE427189T1 (de) | 2009-04-15 |
CN101142056A (zh) | 2008-03-12 |
EP1758713A2 (fr) | 2007-03-07 |
EP1758713A4 (fr) | 2007-10-10 |
CA2566888A1 (fr) | 2005-12-01 |
WO2005112601A2 (fr) | 2005-12-01 |
DE602005013666D1 (de) | 2009-05-14 |
JP2007537891A (ja) | 2007-12-27 |
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