EP1062053A1 - Method for powder-coating - Google Patents
Method for powder-coatingInfo
- Publication number
- EP1062053A1 EP1062053A1 EP99911798A EP99911798A EP1062053A1 EP 1062053 A1 EP1062053 A1 EP 1062053A1 EP 99911798 A EP99911798 A EP 99911798A EP 99911798 A EP99911798 A EP 99911798A EP 1062053 A1 EP1062053 A1 EP 1062053A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- powder
- substrate
- radiation
- temperature
- layer
- 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.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
- B05D3/0263—After-treatment with IR heaters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
- B05D2401/30—Form of the coating product, e.g. solution, water dispersion, powders or the like the coating being applied in other forms than involving eliminable solvent, diluent or dispersant
- B05D2401/32—Form of the coating product, e.g. solution, water dispersion, powders or the like the coating being applied in other forms than involving eliminable solvent, diluent or dispersant applied as powders
Definitions
- the invention relates to a method for powder coating a substrate, in particular a temperature-sensitive substrate such as wood, wood fiber material, plastic, rubber, fabric, paper or cardboard.
- the invention further relates to the use of a halogen lamp for powder coating.
- thermoreactive powder A method for crosslinking thermoreactive powder is known, in which the necessary curing temperature is achieved via multi-stage energy transfers. First, the surface of the powder coating is heated via infrared (IR) radiation or convectively. Only then is the soaking in the powder layer carried out via heat conduction processes up to
- Substrate boundary layer There, the energy, particularly with metallic substrates, is dissipated much faster into the substrate via the higher heat conduction.
- the boundary layer only reaches the necessary crosslinking temperature when the substrate is almost completely warmed up.
- only the temperature gradient between the coating surface and the substrate is the driving process variable for the heating of the coating. In order to ensure homogeneous crosslinking and perfect adhesion to the To ensure substrate, heating times of several minutes are necessary.
- the crosslinking and curing temperatures of powder coatings are often between 120 ° C and 300 ° C. Because of these high temperatures, temperature-sensitive substrates cannot be powder-coated or only to a limited extent by the known method.
- a method for crosslinking and curing a layer of thermoreactive powder on a substrate in which a primer is applied to the surface of the substrate before the thermoreactive powder is applied.
- the primer consists, for example, of water-based paint.
- the primer is used, in particular in the case of substrates made of wood or wood fiber materials, to compensate for inhomogeneities on the surface of the substrate, to form a moisture barrier and to enable the thereactive powder to adhere.
- the powder can then be crosslinked and cured by irradiation with electromagnetic radiation, in particular with medium-wave infrared radiation.
- the primer also forms a heat conduction barrier which prevents heat transfer during the crosslinking reaction in the powder layer to the substrate. This made it possible to apply a powder coating in the first place, especially for temperature-sensitive substrates.
- this known method is limited to the use of thermoreactive powders, the crosslinking temperature of which is only slightly higher than the damage temperature of the substrate.
- the known methods also have the problem that a minimum moisture content of the substrate is desired on the one hand, but on the other hand prevents the application of a uniform powder coating.
- Moisture in the substrate enables, on the one hand, deposit active powder on the charged surface.
- the moisture evaporates in the subsequent crosslinking and curing reaction in the substrate, since, because of the long reaction time at temperatures above the evaporation temperature, the substrate is heated to the evaporation temperature at least on its surface. Therefore, bubbles form on the surface, under the already cross-linked powder, which lead to an irregular layer of lacquer.
- a primer layer does not help here because it does not form a heat conduction barrier that is effective in the long term and because the evaporation temperatures are usually significantly lower than the crosslinking and curing temperatures of the thermoreactive powder.
- the invention has for its object to provide a method for powder coating a substrate, in particular a temperature sensitive substrate such as wood, wood fiber material, plastic, rubber, fabric, paper or cardboard, which allows powder coating of the uncoated surface of the substrate without damaging it, and which leads to an even, completely cross-linked and well-adhering lacquer layer.
- a temperature sensitive substrate such as wood, wood fiber material, plastic, rubber, fabric, paper or cardboard
- An essential idea in the process for powder coating according to the invention is that the required energy is introduced in a targeted and continuous manner over the entire thickness of the powder layer into the amount of powder applied as a base layer to the uncoated surface of the substrate.
- the gelation or crosslinking energy is at least in the form of radiation energy
- the radiation used here has at least radiation components in the near and / or short-wave infrared.
- the powder layer and the substrate surface are preferably heated homogeneously by near infrared radiation (NIR radiation) and in a matter of seconds to the required gelling or crosslinking temperature.
- NIR radiation near infrared radiation
- Near infrared is understood to mean the wavelength range of electromagnetic radiation between the visible range and 1.2 ⁇ m wavelength.
- Short-wave infrared is understood to mean the wavelength range between 1.2 ⁇ m wavelength and 2 ⁇ m wavelength.
- thermo-reactive powder is either heated to the crosslinking temperature and cured by the infrared radiation, or heated to the setting temperature and only crosslinked and cured in a later process step. In the latter case, gelation creates a composite of the powder material without complete crosslinking or curing to form a lacquer layer.
- This also provides excellent controllability of the connection or crosslinking process, in particular since the desired process progress can be controlled precisely by controlling the radiation flux density, the spectral distribution of the radiation energy and / or the radiation duration. It is advantageous if the process parameters mentioned above are based on the absorption tion properties of the thermoreactive powder, on the reflection properties of the substrate surface and on the thermal conductivity of the substrate.
- the rapid, continuous heating of the base layer ensures good adhesion to the substrate surface.
- a second layer of a thermoreactive powder is preferably applied to the hardened or pre-gelled base layer, and the entire not yet fully crosslinked coating is crosslinked and cured by means of the infrared radiation.
- the second layer is applied immediately after curing or pre-gelling.
- the second layer with the application and curing of which the painting process is particularly ended, can produce a uniform paint surface that meets the highest quality requirements.
- irregularities in the base layer are compensated for by the second layer, as a result of which, for example, a uniformly glossy or matt lacquer surface can be achieved.
- matt powder coating surfaces can be achieved with both the first and the second.
- a particularly homogeneous lacquer layer which is crosslinked evenly over the depth of the overall lacquer can form, in particular when using the same type of powder for the base layer and the second layer. The advantages of this powder coating system are therefore particularly evident the robustness, abrasion resistance and chemical resistance of the paint.
- substrates such as wood and wood fiber-containing materials (in short: wood fiber materials) can be powder-coated with a high coating quality.
- wood fiber materials in short: wood fiber materials
- the targeted control of the crosslinking and curing process described above can prevent bubbles of moisture from producing irregularities in the lacquer layer.
- the problem of uneven adhesion of powder particles to an uncoated surface, at least partially formed by wood fibers is overcome.
- An adhesive layer is formed through the base layer, which may still have an irregular surface or even consist of individual, island-like lacquer spots that are not connected to one another. After the base layer has hardened or pre-gelled, however, much better starting conditions exist for the second layer.
- Adhesion is improved and, as a rule, more material is applied when the powder of the second layer is applied. During the subsequent crosslinking and curing of the entire coating material which has not yet been crosslinked or only partially crosslinked, the coating material then runs to form a uniform lacquer layer.
- the powdery base layer and / or the second layer is preferably not irradiated for longer than 12 s, in particular not longer than 8 s, until it gels or hardens. After the application of a second layer, however, the radiation of the base layer is continued by radiation penetrating into the base layer, so that the total radiation duration of the base layer can be longer than 12 or 8 s.
- the surface temperature of the thermoreactive powder is determined in a further development of the method a pyrometer measured and controlled by controlling the radiation flux density of the infrared radiation.
- a pyrometer measured and controlled by controlling the radiation flux density of the infrared radiation.
- a high-performance halogen lamp with a beam temperature of more than 2500 K is preferably used to generate the infrared radiation.
- Such radiation sources generate electromagnetic radiation with very high radiation flux densities, which in particular allow the crosslinking temperature to be reached within a few seconds.
- Incandescent bodies, in particular heating coils, with a low mass are preferably used in the halogen lamp, so that the radiation flux density can be controlled quickly.
- the halogen lamp is combined with a reflector for reflecting the emitted radiation in the direction of the substrate and the halogen lamp is operated in such a way that a maximum radiation flux density of the emitted radiation is in the near infrared.
- the surface temperature of the filament can be adjusted up to 3500 K.
- Line-like halogen lamps are preferably used in combination with trough-like ellipsoidal or parabolic reflectors.
- the uncoated surface of the substrate, in particular of plastic, is expediently pretreated to improve the conductivity for an electrostatic
- thermoreactive powder subjected.
- an electrically conductive liquid is applied to the surface of the substrate.
- a defined moisture content is generated by drying and / or moistening the substrate before applying the base layer. Consequently Particularly uniform powder coating can be achieved and the process parameters can vary within certain limits without reducing the coating quality.
- the substrate surface is irradiated with the same or higher energy input than is necessary for the actual crosslinking process, in particular by NIR radiation.
- This energy input achieves a surface temperature that is above the melting point of the powder system.
- the thermoreactive powder is then applied to the substrate surface as a base layer.
- the thermoreactive powder melts immediately and is optionally crosslinked by continued irradiation.
- the pretreatment of the substrate surface increases the application efficiency many times over during powder application. At the same time, it is prevented that during the actual crosslinking process, moisture accumulated on the substrate surface is expelled, which could disrupt homogeneous film formation.
- Fig. 1 is a medium density fiberboard (MDF) with two layers of powder coating and
- Fig. 2 shows an arrangement for crosslinking powder paint on self-contained peripheral surfaces of a plastic substrate.
- the substrate shown in FIG. 1 consists of a medium-density fiberboard (MDF) 1, which also has a base layer made of thermally active powder and a second layer was coated from thermoreactive powder.
- MDF medium-density fiberboard
- the MDF 1 was grounded on the side not to be coated and the thermoreactive powder of the first lacquer layer 2 was applied to the uncoated surface of the MDF 1 using the tribo process.
- the base layer was then irradiated for 5 s by means of infrared radiation from a radiation source, the maximum radiation flux density of which is about 1 ⁇ m wavelength, until the temperature of the powder has risen to the setting temperature. This temperature, which was approximately homogeneous over the thickness of the first lacquer layer 2, was held for approximately 1 s. The irradiation process was then stopped.
- the substrate had warmed only on its surface and only slightly, so that the water bound in the MDF 1 did not escape at the surface and the uniformity of the coating was not disturbed.
- the MDF 1 was grounded on the uncoated side and thermoreactive powder for the second lacquer layer 3 was applied to the surface of the first lacquer layer 2 using the tribo process.
- the first 2 and the second 3 lacquer layers were then irradiated with the infrared radiation at a maximum radiation flux density with a wavelength of approximately 1 ⁇ until the crosslinking temperature was reached.
- the crosslinking reaction was continued until both coating layers had completely hardened by continued irradiation with a lower radiation flux density for about 3 s. Thereafter, the radiation was stopped and a few seconds waited until the layers of paint had cooled significantly below the crosslinking temperature.
- the second irradiation process also did not generate any steam or gas bubbles that could have caused the paint coating to be irregular.
- DJ DJ 3 ⁇ - o ⁇ - ⁇ DJ Z iQ ⁇ - a N z hf hf li ⁇ 1 03 H cn ⁇ O T D O
- DJ: o H o DJ 3 ⁇ - hh ⁇ yQ 0 ⁇ - tr o ⁇ - ⁇ ⁇ tr 1 hf h- ' ⁇ ⁇ TJ hf rt h DJ:
- the halogen tube radiators 7 in FIG. 2 have a filament 10 of low mass in a quartz glass tube 11.
- the two ends of the filament 10 are each cooled by inflowing compressed air in order to increase the service life of the halogen tube beam 7.
- the reflector 8 is cooled by means of compressed air or liquid in order to create constant conditions for the reflection of the radiation emitted by the halogen tube emitters 7.
Landscapes
- Application Of Or Painting With Fluid Materials (AREA)
- Paints Or Removers (AREA)
- Coating Apparatus (AREA)
Abstract
Description
Claims
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19811319 | 1998-03-16 | ||
DE19811319 | 1998-03-16 | ||
DE1998131781 DE19831781A1 (en) | 1998-07-15 | 1998-07-15 | Accelerated powder-coating of temperature-sensitive materials, e.g. wood, plastic, rubber, material, paper or card |
DE19831781 | 1998-07-15 | ||
PCT/EP1999/001720 WO1999047276A1 (en) | 1998-03-16 | 1999-03-16 | Method for powder-coating |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1062053A1 true EP1062053A1 (en) | 2000-12-27 |
EP1062053B1 EP1062053B1 (en) | 2002-08-14 |
Family
ID=26044646
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP99911798A Revoked EP1062053B1 (en) | 1998-03-16 | 1999-03-16 | Method for powder-coating |
Country Status (11)
Country | Link |
---|---|
US (1) | US6436485B1 (en) |
EP (1) | EP1062053B1 (en) |
JP (1) | JP2002506725A (en) |
KR (1) | KR100685477B1 (en) |
CN (1) | CN1203924C (en) |
AU (1) | AU3035299A (en) |
BR (1) | BR9908843A (en) |
CA (1) | CA2324097A1 (en) |
DE (1) | DE59902341D1 (en) |
ES (1) | ES2182500T3 (en) |
WO (1) | WO1999047276A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1252938A2 (en) * | 2001-04-18 | 2002-10-30 | Rohm And Haas Company | Differential processing of substrates before powder coating the substrate |
Families Citing this family (41)
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DE19834184A1 (en) * | 1998-07-29 | 2000-02-03 | Basf Ag | Process and device for optimizing paints |
DE19857045C2 (en) * | 1998-12-10 | 2001-02-01 | Industrieservis Ges Fuer Innov | Coating of objects |
DE19913446C2 (en) * | 1999-03-25 | 2002-10-31 | Herberts Gmbh & Co Kg | Process for multi-layer painting |
DE19947350C1 (en) * | 1999-10-01 | 2001-01-25 | Industrieservis Ges Fuer Innov | Molding of parts with surface structure, e.g. for vehicle dashboard trim, involves heating with infra-red radiation through transparent mold |
CA2321514A1 (en) * | 1999-10-15 | 2001-04-15 | Gerald K. White | Multiple layered coating on heat-sensitive substrates |
DE10009822C1 (en) * | 2000-03-01 | 2001-12-06 | Basf Coatings Ag | Process for the production of coatings, adhesive layers or seals for primed or unprimed substrates and substrates |
DE10024731A1 (en) * | 2000-05-08 | 2001-11-22 | Advanced Photonics Tech Ag | Manufacturing arrangement for thin-film layer structure, having supply and layer application arrangement, and near-infrared irradiation arrangement |
EP1186952A1 (en) * | 2000-09-06 | 2002-03-13 | Fuji Photo Film B.V. | Method of coating a continuously moving web |
WO2002026897A2 (en) * | 2000-09-29 | 2002-04-04 | Advanced Photonics Technologies Ag | Method and arrangement for producing a coated thermosensitive article or container with thermosensitive contents |
DE10048361C1 (en) * | 2000-09-29 | 2002-06-06 | Advanced Photonics Tech Ag | Arrangement for producing a coated heat-sensitive article or a container with a heat-sensitive content comprises a radiation source producing infrared radiation with an effective constituent in the near-infrared range |
AU2002223671A1 (en) * | 2000-11-08 | 2002-05-21 | Adphos Advanced Photonics Technologies Ag | Method for generating a coating on a substrate |
US6821575B2 (en) | 2000-12-21 | 2004-11-23 | Advanced Photonics Technologies Ag | Electrode treatment |
DE10125888C2 (en) * | 2001-04-18 | 2003-03-13 | Advanced Photonics Tech Ag | Spotlight module and high-performance radiation system |
ES2182715B1 (en) * | 2001-07-24 | 2004-08-16 | Jesus Francisco Barberan Latorre | AUTOMATIC MACHINE FOR THE VARNISHING OF WOOD, MDF, OR AGLOMERATED FLAT PARTS, WITH ULTRAVIOLET POWDER. |
US20040219385A1 (en) * | 2002-08-23 | 2004-11-04 | Rene Mattern | Process for curing powder coatings |
DE20221980U1 (en) | 2002-09-26 | 2009-12-17 | Advanced Photonics Technologies Ag | Arrangement for the thermal treatment of a workpiece |
MXPA05003691A (en) | 2002-10-07 | 2005-11-17 | James Hardie Int Finance Bv | Durable medium-density fibre cement composite. |
US20040265504A1 (en) * | 2003-06-27 | 2004-12-30 | Christophe Magnin | Non-metalic substrate having an electostatically applied activatable powder adhesive |
WO2005037451A1 (en) * | 2003-10-21 | 2005-04-28 | Climate Coating Limited | Powder coating procedures |
US20050095353A1 (en) * | 2003-10-31 | 2005-05-05 | Franziska Isele | Method of curing powder coatings |
NZ548221A (en) | 2004-01-12 | 2010-06-25 | Hardie James Technology Ltd | Composite fibre cement article with radiation curable component |
US20050255238A1 (en) * | 2004-05-12 | 2005-11-17 | Myer Charles N | Pulsed heating process for curing substrates with near infrared radiation |
US20050276917A1 (en) * | 2004-06-15 | 2005-12-15 | Helene Bolm | Process for the preparation of powder coatings |
US7998571B2 (en) * | 2004-07-09 | 2011-08-16 | James Hardie Technology Limited | Composite cement article incorporating a powder coating and methods of making same |
EP1781750A4 (en) * | 2004-07-27 | 2012-08-08 | Duluxgroup Australia Pty Ltd | System for providing powder coated reconstituted cellulosic substrate |
GB2428395B (en) * | 2005-07-19 | 2007-09-05 | Ian Webb | A process of powder coating and a powder coating apparatus |
US20070077435A1 (en) * | 2005-10-05 | 2007-04-05 | Schachter Deborah M | Process for coating a medical device |
US20070111007A1 (en) * | 2005-11-14 | 2007-05-17 | Uwe Wilkenhoener | Process for the preparation of coatings with specific surface properties |
WO2007065222A1 (en) | 2005-12-07 | 2007-06-14 | Depco-Trh Pty Ltd | Pre-preg and laminate manufacture |
SI1810755T1 (en) * | 2006-01-21 | 2009-12-31 | Rich Cup Bio Chemical Technolo | Method to make vessel with heat insulation surface layer |
MX2008013202A (en) | 2006-04-12 | 2009-01-09 | James Hardie Int Finance Bv | A surface sealed reinforced building element. |
DE102006032111A1 (en) * | 2006-07-11 | 2008-01-24 | Tgc Technologie-Beteiligungsgesellschaft Mbh | Radiation apparatus, method and arrangement for powder coating wood-based materials |
DE102006044959B4 (en) * | 2006-09-22 | 2012-04-12 | Wd Beteiligungs Gmbh | Method and apparatus for powder coating wood substrates |
DE102007015261A1 (en) | 2007-03-27 | 2008-10-02 | Aacure Aadhesives Gmbh | Reactive mass for substrate application, preferably for the generation of a glop-top, comprises a thermally initiable matrix forming material and an energy absorbing initiator, where the initiator is soluble in the reactive mass |
GB2452545A (en) * | 2007-09-07 | 2009-03-11 | Fira Internat Ltd | Lignocellulose coated with laser fused powder |
CA2840103A1 (en) * | 2011-05-25 | 2012-11-29 | Superl Technology Limited | Methods of powder coating and items to be powder coated |
CN103917345A (en) * | 2011-05-25 | 2014-07-09 | 励泰科技有限公司 | Methods of powder coating and items to be powder coated |
CN106413919A (en) * | 2013-11-28 | 2017-02-15 | 励泰科技有限公司 | Methods of powder coating and items to be powder coated |
KR101675997B1 (en) * | 2015-07-16 | 2016-11-14 | 주식회사 대마 | Non-conductive powder coating panels and the panels production method |
WO2018132109A1 (en) | 2017-01-15 | 2018-07-19 | Hewlett-Packard Development Company, L.P. | Reflector assembly with partial elliptical cavities |
WO2018190844A1 (en) * | 2017-04-13 | 2018-10-18 | Hewlett-Packard Development Company, L.P. | Reflective barriers |
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GB2024658A (en) * | 1978-07-07 | 1980-01-16 | Shaw J G | Coating of compressed board materials |
GB2056885A (en) | 1979-08-08 | 1981-03-25 | Blundell Permoglaze Ltd | Powder coating cellulose fibre substrates |
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JPH0792831A (en) * | 1993-08-11 | 1995-04-07 | Kiyotsukou Seiko Kk | Infrared-ray irradiating method using halogen lamp |
JPH0777894A (en) * | 1993-08-11 | 1995-03-20 | Kiyotsukou Seiko Kk | Method for retreating thermal radiation fixing part in electrophotographic printer |
AU1263695A (en) * | 1993-12-13 | 1995-07-03 | Electrostatic Technology, Inc. | Powder coating method for producing a composite web |
DE19533858B4 (en) * | 1995-09-13 | 2005-09-22 | IHD Institut für Holztechnologie Dresden gGmbH | Process for the electrostatic coating of wood and wood-based materials |
JPH09201517A (en) * | 1996-01-30 | 1997-08-05 | Inax Corp | Membrane unit |
-
1999
- 1999-03-16 KR KR1020007010216A patent/KR100685477B1/en not_active IP Right Cessation
- 1999-03-16 JP JP2000536498A patent/JP2002506725A/en not_active Withdrawn
- 1999-03-16 CA CA002324097A patent/CA2324097A1/en not_active Abandoned
- 1999-03-16 CN CNB998040533A patent/CN1203924C/en not_active Expired - Fee Related
- 1999-03-16 WO PCT/EP1999/001720 patent/WO1999047276A1/en active IP Right Grant
- 1999-03-16 AU AU30352/99A patent/AU3035299A/en not_active Abandoned
- 1999-03-16 DE DE59902341T patent/DE59902341D1/en not_active Expired - Fee Related
- 1999-03-16 ES ES99911798T patent/ES2182500T3/en not_active Expired - Lifetime
- 1999-03-16 BR BR9908843-6A patent/BR9908843A/en not_active Application Discontinuation
- 1999-03-16 EP EP99911798A patent/EP1062053B1/en not_active Revoked
- 1999-03-16 US US09/646,324 patent/US6436485B1/en not_active Expired - Fee Related
Non-Patent Citations (1)
Title |
---|
See references of WO9947276A1 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1252938A2 (en) * | 2001-04-18 | 2002-10-30 | Rohm And Haas Company | Differential processing of substrates before powder coating the substrate |
EP1252938A3 (en) * | 2001-04-18 | 2003-11-26 | Rohm And Haas Company | Differential processing of substrates before powder coating the substrate |
Also Published As
Publication number | Publication date |
---|---|
KR20010041912A (en) | 2001-05-25 |
DE59902341D1 (en) | 2002-09-19 |
CN1293598A (en) | 2001-05-02 |
CA2324097A1 (en) | 1999-09-23 |
WO1999047276A1 (en) | 1999-09-23 |
AU3035299A (en) | 1999-10-11 |
CN1203924C (en) | 2005-06-01 |
US6436485B1 (en) | 2002-08-20 |
KR100685477B1 (en) | 2007-02-23 |
ES2182500T3 (en) | 2003-03-01 |
JP2002506725A (en) | 2002-03-05 |
BR9908843A (en) | 2000-11-21 |
EP1062053B1 (en) | 2002-08-14 |
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