EP1173314A2 - Procede et materiau pour la fabrication de corps servant de modeles - Google Patents

Procede et materiau pour la fabrication de corps servant de modeles

Info

Publication number
EP1173314A2
EP1173314A2 EP00926905A EP00926905A EP1173314A2 EP 1173314 A2 EP1173314 A2 EP 1173314A2 EP 00926905 A EP00926905 A EP 00926905A EP 00926905 A EP00926905 A EP 00926905A EP 1173314 A2 EP1173314 A2 EP 1173314A2
Authority
EP
European Patent Office
Prior art keywords
laser
plastic powder
plastic
dyes
dye
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Withdrawn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
EP00926905A
Other languages
German (de)
English (en)
Inventor
Wolfgang Podszun
David Bryan Harrison
Jean-Marie Dewanckele
Frank Louwet
Gabriele Alscher
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.)
Bayer AG
Original Assignee
Bayer AG
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 Bayer AG filed Critical Bayer AG
Publication of EP1173314A2 publication Critical patent/EP1173314A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
    • B29C67/02—Moulding by agglomerating
    • B29C67/04—Sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
    • B29C64/10—Processes of additive manufacturing
    • B29C64/141—Processes of additive manufacturing using only solid materials
    • B29C64/153—Processes of additive manufacturing using only solid materials using layers of powder being selectively joined, e.g. by selective laser sintering or melting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
    • B29C35/0805—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
    • B29C2035/0822—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation using IR radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005—Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/0032—Pigments, colouring agents or opacifiyng agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005—Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/0047—Agents changing thermal characteristics
    • B29K2105/005—Heat sensitisers or absorbers

Definitions

  • the invention relates to a method for the production of model bodies, in which any three-dimensional structure can be built up with the aid of selective sintering using laser light in the IR range using plastics, in the form of selected plastic powders.
  • the invention also relates to a special plastic powder which contains an IR absorber and is particularly well suited for sintering with IR laser light.
  • the invention relates in particular to a method for producing three-dimensional models from plastic in accordance with stored, geometric data with the aid of a computer-assisted system for direct production of prototypes and models (rapid prototyping system) which works with IR laser beams.
  • Rapid prototyping is the term used to summarize the computer-controlled additive, automatic model building methods known today.
  • Laser sintering is a rapid prototyping process in which fillings made of certain powdery materials are heated and sintered in layers at certain plane positions under the influence of laser beams, preferably controlled by a program.
  • plastic powders for laser sintering using CO 2 lasers is known (A. Gebhardt, Rapid Prototyping, Carl Hanser Verlag, Kunststoff, Vienna 1996, pages 115-116).
  • a method for the production of model bodies is described in which, using plastics with the aid of light from a CO laser, any three-dimensional structure can be built up by selective sintering.
  • a disadvantage of the previously known methods is the limited accuracy of the moldings obtained. Because of this inaccuracy, they have to be this way today generated moldings can be manually reworked in a complex manner in many cases.
  • the low accuracy is partly a result of the CO 2 laser used, which has a wavelength of 10.6 ⁇ m and is difficult to focus.
  • better focusable lasers such as the ND-Y AG laser with a wavelength of 1064 nm, have not been used for laser sintering since the usual plastics do not show any absorption at this wavelength.
  • the invention relates to a method for producing three-dimensional models from plastic in accordance with stored geometric data with the aid of laser beams of a wavelength 500 to controlled according to this data
  • the plastic powder is essentially spherical.
  • Another object of the present invention are plastic powders for use as a starting material for laser-assisted production of models, the powder particles having an average particle size (i.e. weight average diameter) of 2 to 200 ⁇ m and containing an IR absorber.
  • the powder particles having an average particle size (i.e. weight average diameter) of 2 to 200 ⁇ m and containing an IR absorber.
  • Solid-state lasers and semiconductor diode lasers are particularly suitable.
  • solid lasers are Nd-YAG lasers with a wavelength of 1064 nm and Nd-YLF lasers with a wavelength of 1053 nm.
  • Diode lasers which emit at 823 nm or 985 nm are mentioned.
  • the irradiated energy on the surface of the powder bed is preferably from 0.01 to 100 mJ / mm 2 , preferably 1 to 50 mJ / mm 2 during the irradiation.
  • the effective diameter of the laser beam is in particular from 0.001 to 0.05 mm, preferably from 0.01 to 0.05 mm.
  • Pulsed lasers are preferably used, a high pulse frequency, in particular from 1 to 100 kHz, having proven particularly suitable.
  • the laser beam strikes the uppermost layer of the bed made of the material to be used according to the invention and melts or sinters the material in a certain layer thickness.
  • This layer thickness can be from 0.005 mm to 1 mm, preferably from 0.01 mm to 0.5 mm.
  • the first layer of the desired component is produced in this way.
  • the working space is then lowered by an amount which is less than the thickness of the sintered layer.
  • the work space is filled up to the original height with additional polymer material.
  • the second layer of the component is sintered and connected to the previous layer. By repeating the process, the additional layers are created until the component is finished.
  • the laser beam is applied at a speed of 1 to 1,000 mm / s, preferably 10 to 100 mm / s.
  • Plastic powders suitable for the invention can belong to different polymer classes. Examples include: polyolefins such as polyethylene and polypropylene, polyamides such as polyamide 6 and polyamide 6,6, polyesters such as polyethylene terephthalate and polybutyl terephthalate, polycarbonates, meltable polyurethanes,
  • Plastic powder on The base of partially crystalline polymers are particularly suitable for the production of pore-free model bodies.
  • the particle size of the powder particles is of particular importance for the process according to the invention. Generally the average particle diameter is 2 to
  • the weight average is meant here as the mean particle diameter (particle size).
  • the plastics which are usually present as coarse granules can be ground. However, this may result in an angular or angular shape of the plastic particles. These particles with an irregular or torn surface sometimes have poor flow properties, which have an unfavorable effect on processing in laser sintering systems. It is therefore usually necessary to add flow aids to the plastics in order to improve the flowability of the shredded plastics and to ensure the operation of automated systems.
  • Polymers with an essentially spherical shape are particularly suitable for the process according to the invention.
  • the bead polymer does not leave any annoying residues when it is incinerated, for example as the core of a hollow ceramic mold. In the case of ground artificial particles mixed with flow aids, it has been observed that these do not incinerate without residues.
  • the plastic models which are primarily created using laser sintering, are further processed in subsequent processes for investment casting. For this purpose, for example after the model produced with the method according to the invention has been coated with wax to further improve the model surface, the model is immersed in a slurried ceramic mass and this with
  • Ceramic coated model fired in the oven The model should burn completely when fired and leave the free hollow shape made of ceramic. Since conventional ground plastics do not burn completely due to the flow aid, the metallic models subsequently cast in the ceramic mold often have surface inaccuracies.
  • the bead polymers preferably consist of homopolymers or copolymers of monoethylenically unsaturated compounds (monomers).
  • Copolymers in the sense of the invention include polymers which consist of two or more different
  • Monomers are built up, understood. Suitable monomers are e.g. Styrene, alpha-methylstyrene, chlorostyrene, acrylic acid esters, such as ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, decyl acrylate, dodecyl acrylate, methacrylic acid esters, such as methyl methacrylate, ethyl methacrylate, isopropyl methacrylate, n-butyl methacrylate, iso-butyl methacrylate, iso-butyl methacrylate, iso-butyl methacrylate, Decyl methacrylate, dodecyl methacrylate, stearyl methacrylate, furthermore acrylonitrile, methacrylonitrile, methacrylamide and vinyl acetate.
  • acrylic acid esters such as ethyl acrylate, butyl acrylate, 2-ethyl
  • the molecular weight of the bead polymers is important for the suitability for the process according to the invention.
  • the molecular weight of the bead polymers is important for the suitability for the process according to the invention.
  • molecular weight regulators can be used in the preparation of the bead polymers. Suitable molecular weight regulators are in particular sulfur compounds, for example n-butyl mercaptan, dodecyl mercaptan, thioglycolic acid ethyl ester and diisopropyl xanthogen disulfide.
  • the sulfur-free regulators mentioned in DE 3 010 373 are also very suitable for adjusting the molecular weight, for example the enol ethers of the formula I.
  • Particularly suitable bead polymers can be prepared by processes known per se. So bead polymers with a particle size of about 10 to 200 can be obtained by suspension polymerization or bead polymerization.
  • suspension polymerization is understood to mean a process in which a monomer or a monomer-containing mixture which is soluble in the monomer (s)
  • Initiator contains, in a phase which is essentially immiscible with the monomer (s) and which contains a dispersant, is divided into droplets, optionally in a mixture with small, solid particles, and is cured by increasing the temperature with stirring. Further details of the suspension polymerization are described, for example, in Ulimann's Encyclopedia of Industrial Chemistry, Vol. A21
  • Bead polymers with particle sizes of 2 to 10 ⁇ m can be produced by the so-called dispersion polymerization.
  • Dispersion polymerization uses a solvent in which the monomers used are soluble but the polymer formed is insoluble.
  • Dispersion polymerization generally provides bead polymers with a narrow particle size distribution. In principle, all compounds which absorb light at a wavelength of 500 to 1500 nm, preferably 800 to 1200 nm, are suitable as IR absorbers. Both IR pigments and IR dyes can be used independently of one another.
  • Carbon black, in particular synthetically produced carbon black, is particularly suitable as the IR pigment.
  • the carbon black preferably has a specific surface area of 10 to 500 m 2 / g, measured by the BET method.
  • Suitable types of carbon black are gas blacks (channel blacks), furnace blacks (furnace blacks) and lamp blacks.
  • mixed metal oxide pigments of the rutile or spinel type are well suited.
  • suitable metal oxide pigments are the commercially available products HEUCODUR ® -Brown 859 and HEUCODUR ® -Black 953.
  • IR dyes infra-red absorbing dyes, IRD
  • IRD infra-red absorbing dyes
  • IR dyes from different substance classes are preferably suitable, e.g. Indoaniline dyes, oxonol dyes, porphine derivatives, antrachinone dyes, mesostyryl dyes, pyrilium compounds and squarylium derivatives.
  • IR dyes according to the published patent application DE 4 331 162 are also particularly suitable, since they have no or only a slight absorption in the visible range and thus enable the production of uncolored or only slightly colored 3D models by the process according to the invention.
  • the IR dye according to formula II may be mentioned as an example:
  • the amount of IR absorber according to the invention is from 0.01 to 10% by weight, preferably from 0.05 to 5% by weight, based on the plastic powder.
  • Plastic powder containing an IR absorber can be produced in different ways. It is thus possible to mix the plastic with the LR absorber in the melt using an extruder and to break the extrudate obtained into the desired particle size in a mill. It is also possible to add the IR absorber during the manufacture of the plastic so that the LR absorber is enclosed in the plastic that is being formed. In the preparation of bead polymers by suspension polymerization, the IR absorber can be added to the monomers.
  • Dyes can be doped.
  • the plastic particles are dispersed in a liquid phase which does not dissolve the plastic, preferably in water, it being possible for a wetting agent or a surfactant to be used.
  • suitable surfactants are, for example, sodium alkyl sulfonate, isooctyl sodium sulfosuccinate or ethoxylated nonylphenol.
  • a solution of the IR dye is added to the dispersion obtained, it being possible preferably to use a water-immiscible solvent, such as, for example, ethyl acetate, toluene, butanone, chloroform, dichloroethane or methyl isobutyl ether.
  • the solvent including the IR dye, swells in the plastic particles.
  • the water can then be filtered or animals and the solvent by evaporation, e.g. B are removed at reduced pressure, the IR dye remaining in the plastic particle.
  • the plastic powders according to the invention which contain an IR absorber, are particularly well suited for the laser sintering process with LR lasers, in particular ND-YAG lasers, and deliver models or components with particularly good attention to detail.
  • Figure 1 shows the schematic representation of a rapid prototyping system.
  • Bead polymer 200 g of the dispersion from a) and 2.0 g of 2,2'-azobis (isobutyronitrile) were mixed intensively.
  • the mixture is transferred to a stirred reactor which has previously been treated with 1.0 liter of a 1% strength by weight aqueous alkaline solution of a copolymer of 50% by weight methacrylic acid and 50% by weight adjusted to pH 8 with sodium hydroxide solution .-% methyl methacrylate was filled.
  • the stirring speed was set to 700 revolutions per minute and the temperature was kept at 60 ° C. for 3 hours, then at 78 ° C. for 10 hours and then at 85 ° C. for 2 hours.
  • the mixture was then cooled to room temperature within 2 hours.
  • the bead polymer formed was isolated by decanting, washed several times with water and dried at 50 ° C. in vacuo. 168 g of an intensely black-colored bead polymer with an average particle size of 18 ⁇ m and a molecular weight Mw of 230,000 were obtained.
  • the bead polymer formed was isolated by decanting, washed several times with water and dried at 50 ° C. in vacuo. 205 g of an intensely black-colored bead polymer with an average particle size of 25 ⁇ m and a molecular weight Mw of 220,000 were obtained.
  • 64 g of polyvinylpyrrolidone, 240 g of styrene and 60 g of ethyl methacrylate are mixed to form a homogeneous solution.
  • This solution was brought to 70 ° C. in the course of one hour under nitrogen at a stirring speed of 100 rpm and a solution of 3.75 g of 2,2'-azobis (isobutyronitrile) in 75 g of styrene was added to the reactor.
  • the polymerization mixture was stirred for a further 15 hours at 70 ° C. and 100 rpm.
  • the polymer dispersion formed was then cooled to room temperature and the bead polymer was isolated by sedimentation. 247 g of bead polymer were obtained with an average particle size of 14 ⁇ m and a 0 (90) / 0 ( ⁇ ) value of 1.6 and a molecular weight Mw of 60,000.
  • the beam of an ND-YAG laser 1 (effective cross section 5 mm 2 , pulse frequency 10 Hz) is directed via the deflecting mirror 2 at a speed of 10 mm / s onto the surface of the bed 3 of the bead polymer and an area of 20 x 20 with the laser beam mm scanned.
  • the radiated energy was 40 mJ / mm 2 .
  • Hard beads were obtained with the bead polymers from Examples 1b), 2b), 3b) and 4b).
  • the test baskets were broken mechanically in liquid nitrogen and the fracture surfaces were examined in a scanning electron microscope. In the case of the bead polymer from Example 3a) (comparative experiment, without IR absorber), the product remained unchanged as a powder.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Au moyen de lasers IR, des corps de forme quelconque servant de modèles peuvent être produits par frittage sélectif, à partir de poudres spéciales de matière plastique. On décrit en outre des poudres de matière plastique renfermant un absorbeur IR et utilisées pour la production de modèles assistée au laser.
EP00926905A 1999-04-27 2000-04-13 Procede et materiau pour la fabrication de corps servant de modeles Withdrawn EP1173314A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19918981A DE19918981A1 (de) 1999-04-27 1999-04-27 Verfahren und Material zur Herstellung von Modellkörpern
DE19918981 1999-04-27
PCT/EP2000/003316 WO2000064653A2 (fr) 1999-04-27 2000-04-13 Procede et materiau pour la fabrication de corps servant de modeles

Publications (1)

Publication Number Publication Date
EP1173314A2 true EP1173314A2 (fr) 2002-01-23

Family

ID=7905937

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00926905A Withdrawn EP1173314A2 (fr) 1999-04-27 2000-04-13 Procede et materiau pour la fabrication de corps servant de modeles

Country Status (14)

Country Link
EP (1) EP1173314A2 (fr)
JP (1) JP2002542080A (fr)
KR (1) KR20010114248A (fr)
CN (1) CN1348408A (fr)
AU (1) AU4548200A (fr)
BR (1) BR0010074A (fr)
CA (1) CA2371181A1 (fr)
CZ (1) CZ20013851A3 (fr)
DE (1) DE19918981A1 (fr)
HK (1) HK1046116A1 (fr)
IL (1) IL145779A0 (fr)
MX (1) MXPA01010931A (fr)
TR (1) TR200102922T2 (fr)
WO (1) WO2000064653A2 (fr)

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DE102004009234A1 (de) * 2004-02-26 2005-09-15 Degussa Ag Polymerpulver mit Rußpartikeln, Verfahren zu dessen Herstellung und Formkörper, hergestellt aus diesem Polymerpulver
DE102004012682A1 (de) * 2004-03-16 2005-10-06 Degussa Ag Verfahren zur Herstellung von dreidimensionalen Objekten mittels Lasertechnik und Auftragen eines Absorbers per Inkjet-Verfahren
DE102004012683A1 (de) * 2004-03-16 2005-10-06 Degussa Ag Lasersintern mit Lasern mit einer Wellenlänge von 100 bis 3000 nm
DE102004020452A1 (de) * 2004-04-27 2005-12-01 Degussa Ag Verfahren zur Herstellung von dreidimensionalen Objekten mittels elektromagnetischer Strahlung und Auftragen eines Absorbers per Inkjet-Verfahren
DE102004062761A1 (de) * 2004-12-21 2006-06-22 Degussa Ag Verwendung von Polyarylenetherketonpulver in einem dreidimensionalen pulverbasierenden werkzeuglosen Herstellverfahren, sowie daraus hergestellte Formteile
GB2422344B (en) * 2005-01-24 2008-08-20 Univ Montfort Rapid prototyping method using infrared sintering
DE102006009095A1 (de) * 2006-02-28 2007-08-30 Bayerische Motoren Werke Ag Verfahren zur Herstellung eines beschichteten Formkörpers
JP2010184412A (ja) * 2009-02-12 2010-08-26 Aspect Inc 積層造形用樹脂粉末
WO2014158106A1 (fr) * 2013-03-26 2014-10-02 Nihat Aydin Système de formation de couche à partir d'un métal en fusion directe
CN103772870B (zh) * 2014-01-07 2018-04-27 合肥杰事杰新材料股份有限公司 一种丙烯酸酯类微球改性材料及其制备方法与其在3d打印中的应用
CN103772837A (zh) * 2014-01-08 2014-05-07 合肥杰事杰新材料股份有限公司 一种用于3d打印的聚苯乙烯微球材料及其制备方法
CN103772838B (zh) * 2014-01-08 2018-09-28 合肥杰事杰新材料股份有限公司 一种水滑石改性聚苯乙烯微球材料与制备方法及其在3d打印中的应用
CN103772877B (zh) * 2014-01-08 2018-09-28 合肥杰事杰新材料股份有限公司 一种用于3d打印的聚苯乙烯微球改性光敏树脂及其制备方法
PL412719A1 (pl) * 2015-06-17 2016-12-19 Sinterit Spółka Z Ograniczoną Odpowiedzialnością Kompozycja proszku i sposób wytwarzania trójwymiarowych obiektów metodą selektywnego spiekania lub/i topienia
EP3365156B1 (fr) 2015-10-22 2024-03-27 Dow Global Technologies LLC Procédé de fabrication additive par frittage sélectif et poudre utilisée à cet égard
EP3439853A4 (fr) * 2016-04-05 2019-12-11 Hewlett-Packard Development Company, L.P. Ensembles de matériaux photosensibles
CN108602262B (zh) * 2016-04-11 2021-07-30 惠普发展公司，有限责任合伙企业 颗粒状构建材料
WO2018080537A1 (fr) 2016-10-31 2018-05-03 Hewlett-Packard Development Company, L.P. Imprimante 3d comprenant un agent d'absorption de lumière uv
US10974498B2 (en) 2016-12-28 2021-04-13 Covestro Deutschland Ag Additive fabrication process with a structural material comprising an IR absorber
EP3495155A1 (fr) * 2017-12-08 2019-06-12 Agfa Nv Traitement laser infrarouge proche (nir) des articles en résine
EP3594008A1 (fr) * 2018-07-10 2020-01-15 Agfa-Gevaert Nv Traitement laser infrarouge proche (nir) d'articles à base de résine
DE102018213675A1 (de) 2018-08-14 2020-02-20 Eos Gmbh Electro Optical Systems Additive Herstellvorrichtung und zugeordnetes additives Herstellverfahren

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Also Published As

Publication number Publication date
MXPA01010931A (es) 2002-06-21
CN1348408A (zh) 2002-05-08
WO2000064653A2 (fr) 2000-11-02
CA2371181A1 (fr) 2000-11-02
TR200102922T2 (tr) 2002-02-21
HK1046116A1 (zh) 2002-12-27
DE19918981A1 (de) 2000-11-02
JP2002542080A (ja) 2002-12-10
AU4548200A (en) 2000-11-10
BR0010074A (pt) 2002-01-15
KR20010114248A (ko) 2001-12-31
IL145779A0 (en) 2002-07-25
CZ20013851A3 (cs) 2002-03-13
WO2000064653A3 (fr) 2001-03-29

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