FR2821011A1 - Polymer component surface treatment procedure consists of coarse structuring followed by plasma or flame treatment - Google Patents
Polymer component surface treatment procedure consists of coarse structuring followed by plasma or flame treatment Download PDFInfo
- Publication number
- FR2821011A1 FR2821011A1 FR0202268A FR0202268A FR2821011A1 FR 2821011 A1 FR2821011 A1 FR 2821011A1 FR 0202268 A FR0202268 A FR 0202268A FR 0202268 A FR0202268 A FR 0202268A FR 2821011 A1 FR2821011 A1 FR 2821011A1
- Authority
- FR
- France
- Prior art keywords
- treatment
- plasma
- followed
- structuring
- polymer component
- 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
- 229920000642 polymer Polymers 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000011282 treatment Methods 0.000 title claims abstract description 17
- 238000004381 surface treatment Methods 0.000 title claims description 7
- 238000009832 plasma treatment Methods 0.000 claims abstract description 7
- 238000005553 drilling Methods 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 238000006748 scratching Methods 0.000 claims abstract description 5
- 230000002393 scratching effect Effects 0.000 claims abstract description 5
- 238000003801 milling Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 230000005855 radiation Effects 0.000 abstract 2
- 239000011230 binding agent Substances 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 1
- 239000004812 Fluorinated ethylene propylene Substances 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- 239000004813 Perfluoroalkoxy alkane Substances 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000013532 laser treatment Methods 0.000 description 1
- 229920009441 perflouroethylene propylene Polymers 0.000 description 1
- 229920011301 perfluoro alkoxyl alkane Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/14—Surface shaping of articles, e.g. embossing; Apparatus therefor by plasma treatment
-
- 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
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/02—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing
-
- 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
- B29C2035/0838—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 laser
-
- 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
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/14—Surface shaping of articles, e.g. embossing; Apparatus therefor by plasma treatment
- B29C2059/145—Atmospheric plasma
-
- 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
- B29C2791/00—Shaping characteristics in general
- B29C2791/001—Shaping in several steps
-
- 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
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/08—Surface shaping of articles, e.g. embossing; Apparatus therefor by flame treatment ; using hot gases
-
- 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
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/16—Surface shaping of articles, e.g. embossing; Apparatus therefor by wave energy or particle radiation, e.g. infrared heating
-
- 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
- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
- B29K2027/12—Use of polyvinylhalogenides or derivatives thereof as moulding material containing fluorine
- B29K2027/18—PTFE, i.e. polytetrafluorethene, e.g. ePTFE, i.e. expanded polytetrafluorethene
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Mechanical Engineering (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
Description
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La présente invention concerne un procédé de traitement de surface d'une pièce ou élément de construction en polymère, et la pièce en polymère obtenue par ce procédé. The present invention relates to a method of surface treatment of a polymer part or building element, and the polymer part obtained by this method.
Un procédé de ce type est connu par exemple par le document DE 26 16 466. A process of this type is known for example from document DE 26 16 466.
Il est délicat de coller, revêtir ou imprimer sans pré-traitement les polymères, notamment le polytétrafluoroéthylène (PTFE), et en particulier il est délicat de lier ces polymères avec d'autres matériaux sans pré-traitement. Pour le traitement de surface, on dispose de procédés chimiques dans lesquels le polymère est attaqué avec des solutions de métaux alcalins agressifs, ce qui conduit à la formation d'une couche adhésive à la surface du polymère. Toutefois, un tel procédé est délicat à mettre en oeuvre car les solutions sont susceptibles de conduire à des explosions et sont polluantes. It is difficult to paste, coat or print polymers without pretreatment, in particular polytetrafluoroethylene (PTFE), and in particular it is delicate to bind these polymers with other materials without pretreatment. For surface treatment, chemical processes are available in which the polymer is attacked with solutions of aggressive alkali metals, which leads to the formation of an adhesive layer on the surface of the polymer. However, such a process is difficult to implement because the solutions are liable to lead to explosions and are polluting.
Il est connu également de rendre rugueux des polymères par sablage ou traitement avec des abrasifs. Cependant, au cours de ces traitements, des grains de sable ou d'abrasif pénètrent dans les polymères, ce qui conduit à une structure superficielle indéfinie et à une adhérence insuffisante avec un adhésif. Dans le cas du PTFE, le sablage ou le traitement avec un abrasif n'améliore l'adhérence que de manière négligeable du fait de l'encrassement de la surface de la pièce en PTFE. It is also known to roughen polymers by sandblasting or treatment with abrasives. However, during these treatments, grains of sand or abrasive penetrate into the polymers, which leads to an indefinite surface structure and to insufficient adhesion with an adhesive. In the case of PTFE, sandblasting or treatment with an abrasive improves adhesion only negligibly due to the fouling of the surface of the PTFE part.
Par le document DE 26 16 466, on connaît un procédé de traitement de surface d'une pièce constituée par un polymère d'oléfine fluorée, dans lequel la pièce est exposée à une décharge électrique par application d'une tension alternative entre une cathode et une anode, la pièce étant reliée à la cathode. Une pression de l'atmosphère environnante d'environ 0,066 à 0,66 x 102 Pa (0,0005 à 0,5 torr) est maintenue pendant la décharge de sorte que la pièce est soumise à une attaque par pulvérisation dans la chambre noire cathodique qui se forme. Document DE 26 16 466 discloses a method of surface treatment of a part constituted by a fluorinated olefin polymer, in which the part is exposed to an electric discharge by application of an alternating voltage between a cathode and an anode, the part being connected to the cathode. A pressure of the surrounding atmosphere of about 0.066 to 0.66 x 102 Pa (0.0005 to 0.5 torr) is maintained during the discharge so that the part is subjected to spray attack in the cathode darkroom which is formed.
Ce procédé est proposé à titre d'alternative à un traitement de surface qui consiste par exemple à rendre la surface rugueuse par des moyens mécaniques, car il est indiqué qu'un tel traitement de surface améliore de manière négligeable la surface de pièces constituées par exemple par du polytétrafluoroéthylène (page 1, ligne 45 de DE 26 16 466 C2). This method is proposed as an alternative to a surface treatment which consists, for example, of making the surface rough by mechanical means, since it is indicated that such a surface treatment negligibly improves the surface of parts made up for example with polytetrafluoroethylene (page 1, line 45 of DE 26 16 466 C2).
La présente invention a pour but de proposer un procédé de pré-traitement de la surface d'un polymère grâce auquel il soit possible de The object of the present invention is to propose a process for pre-treating the surface of a polymer by means of which it is possible to
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revêtir ou de lier durablement et solidement un polymère avec d'autres matériaux et qui permette d'obtenir des forces d'adhésion les plus élevées possibles. to coat or bind a polymer durably and securely with other materials and which makes it possible to obtain the highest possible adhesion forces.
Ce but est atteint selon l'invention par un procédé de prétraitement de surface d'une pièce en polymère dans lequel, dans une première étape, la surface de la pièce en polymère est structurée grossièrement au moins par segments et, dans une deuxième étape, la surface structurée grossièrement est soumise à un traitement à plasma ou à un traitement à la flamme. This object is achieved according to the invention by a process of surface pretreatment of a polymer part in which, in a first step, the surface of the polymer part is roughly structured at least by segments and, in a second step, the roughly structured surface is subjected to a plasma treatment or a flame treatment.
Grâce à la structuration grossière de la surface du polymère, la surface de la pièce en polymère qui doit être revêtue, imprimée, collée ou vulcanisée est agrandie efficacement, ce qui permet d'augmenter l'adhérence d'un liant ou adhésif, par exemple. Comme structuration, on peut envisager par exemple des rayures, des rainures, des tranchées, des perçages et d'autres évidements. Le liant peut pénétrer dans ces évidements et s'y fixer solidement lorsqu'il durcit. Il en résulte un ancrage mécanique du liant dans la pièce en polymère. Le fait qu'au cours d'un procédé de traitement à plasma le gaz de traitement puisse pénétrer dans ces évidements constitue un avantage supplémentaire découlant de la formation de tels évidements. Le plasma active la surface en formant dans celle-ci des sites radicalaires qui ont pour effet que la surface du polymère en contact avec le liant ou un revêtement réagit. Plus la surface est agrandie par la structuration grossière, plus la surface active est grande et meilleure est l'adhérence du liant ou de l'adhésif. Au bout d'une durée d'environ 1 min du traitement à plasma, on observe déjà une activation de la surface. La surface est attaquée quand ce traitement est mis en oeuvre pendant des durées plus longues. Dans ce cas, il y a enlèvement de matière. Au bout de 30 min environ, la surface déjà structurée grossièrement subit un profilage supplémentaire qui conduit à une structuration fine de la structure grossière. Ceci augmente encore la surface de contact pour le liant ou l'adhésif de même que la surface active. Thanks to the coarse structure of the polymer surface, the surface of the polymer part which must be coated, printed, glued or vulcanized is effectively enlarged, which makes it possible to increase the adhesion of a binder or adhesive, for example . As structuring, one can consider for example stripes, grooves, trenches, holes and other recesses. The binder can penetrate into these recesses and be fixed there securely when it hardens. This results in mechanical anchoring of the binder in the polymer part. The fact that during a plasma treatment process the treatment gas can penetrate into these recesses constitutes an additional advantage arising from the formation of such recesses. The plasma activates the surface by forming in it radical sites which have the effect that the surface of the polymer in contact with the binder or a coating reacts. The more the surface is enlarged by the coarse structuring, the larger the active surface and the better the adhesion of the binder or the adhesive. After approximately 1 min of the plasma treatment, activation of the surface is already observed. The surface is attacked when this treatment is carried out for longer periods. In this case, there is removal of material. After approximately 30 min, the already roughly structured surface undergoes additional profiling which leads to fine structuring of the coarse structure. This further increases the contact surface for the binder or adhesive as well as the active surface.
Le traitement à plasma peut être mis en oeuvre avec un plasma basse pression ou avec un plasma à la pression atmosphérique (corona). The plasma treatment can be carried out with a low pressure plasma or with a plasma at atmospheric pressure (corona).
A titre d'alternative à l'activation de la surface par un procédé de As an alternative to activating the surface by a process
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traitement à plasma, il est possible également de mettre en oeuvre un procédé de traitement à la flamme. plasma treatment, it is also possible to implement a flame treatment process.
Les polymères qui peuvent être traités par le procédé selon l'invention peuvent être par exemple des matières plastiques comme le
PE, le PP, le POM, le PPS, des polyfluorocarbures comme le PTFE, le PFA, le FEP et des élastomères comme EPDM, NBR et FKM. The polymers which can be treated by the process according to the invention can for example be plastics such as
PE, PP, POM, PPS, polyfluorocarbons like PTFE, PFA, FEP and elastomers like EPDM, NBR and FKM.
On peut aussi réaliser la structuration fine au moyen d'un traitement à laser. Fine structuring can also be carried out using laser treatment.
De préférence, la structuration grossière est réalisée par un traitement mécanique de la pièce en polymère, en particulier par rayure, fraisage, perçage, pressage ou irradiation laser. La structuration est réalisée sur la pièce en polymère terminée. La rayure peut être réalisée par exemple au moyen de couteaux ou d'aiguilles. Pour le pressage, il est possible de prévoir par exemple une planche à clous. Les perçages peuvent être obtenus avec des perceuses conventionnelles ou des perceuses à laser. Les évidements ainsi obtenus ont de préférence une profondeur de 0,05 à 1 mm. Preferably, the rough structuring is carried out by mechanical treatment of the polymer part, in particular by scratching, milling, drilling, pressing or laser irradiation. The structuring is carried out on the finished polymer part. The scratching can be carried out for example by means of knives or needles. For pressing, it is possible to provide for example a nail board. The holes can be obtained with conventional drills or laser drills. The recesses thus obtained preferably have a depth of 0.05 to 1 mm.
Il est possible aussi de réaliser la structuration grossière de la surface de la pièce en polymère au cours de sa fabrication. Dans ce cas, la pièce en polymère peut être munie d'une surface profilée au cours du moulage par injection, du frittage ou de la vulcanisation du polymère, et les outils de mise en forme doivent être structurés de manière correspondante. L'avantage de cette variante réside dans le fait qu'aucune opération supplémentaire n'est nécessaire pour la structuration grossière de la surface de la pièce et que la structuration grossière est très reproductible. It is also possible to carry out the rough structuring of the surface of the polymer part during its manufacture. In this case, the polymer part can be provided with a profiled surface during injection molding, sintering or vulcanization of the polymer, and the shaping tools must be structured correspondingly. The advantage of this variant lies in the fact that no additional operation is necessary for the rough structuring of the surface of the part and that the rough structuring is very reproducible.
Comme gaz de procédé, on peut envisager tous les gaz de procédé courants, en particulier H2, CO, Ar, NH3, 02, N2, de même que HCOOH. As process gas, all common process gases can be considered, in particular H2, CO, Ar, NH3, 02, N2, as well as HCOOH.
La présente invention concerne également une pièce en polymère traitée par le procédé selon l'invention. The present invention also relates to a polymer part treated by the method according to the invention.
Claims (4)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10108456A DE10108456B4 (en) | 2001-02-22 | 2001-02-22 | Surface pretreatment process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| FR2821011A1 true FR2821011A1 (en) | 2002-08-23 |
| FR2821011B1 FR2821011B1 (en) | 2005-02-25 |
Family
ID=7675062
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR0202268A Expired - Fee Related FR2821011B1 (en) | 2001-02-22 | 2002-02-22 | METHOD FOR SURFACE TREATMENT OF A POLYMER PART AND POLYMER PART THUS OBTAINED |
Country Status (3)
| Country | Link |
|---|---|
| DE (1) | DE10108456B4 (en) |
| FR (1) | FR2821011B1 (en) |
| IT (1) | ITTO20020151A1 (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2433406A1 (en) * | 1978-07-27 | 1980-03-14 | Shinetsu Chemical Co | PROCESS FOR IMPROVING PVC RESIN PHONOGRAPH DISCS |
| EP0136918A2 (en) * | 1983-10-04 | 1985-04-10 | Shin-Etsu Chemical Co., Ltd. | A sheet material of a vinyl chloride-based resin having improved surface properties |
| JPH0834865A (en) * | 1994-07-25 | 1996-02-06 | Kanegafuchi Chem Ind Co Ltd | Method for improving adherence of polyimide film and polyimide film improved in adherence |
| US5861192A (en) * | 1995-08-03 | 1999-01-19 | Kanegafuchi Kagaku Kogyo Kabushiki Kaisha | Method of improving adhesive property of polyimide film and polymidefilm having improved adhesive property |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51125455A (en) * | 1975-04-14 | 1976-11-01 | Jiyunkichi Nakai | Method of surface treatment of molded article |
| DE4041884A1 (en) * | 1990-12-27 | 1992-07-02 | Abb Patent Gmbh | METHOD FOR TREATING SURFACES |
| US5374456A (en) * | 1992-12-23 | 1994-12-20 | Hughes Aircraft Company | Surface potential control in plasma processing of materials |
| DE19903479C2 (en) * | 1999-01-29 | 2003-03-20 | Schott Glas | Process for attaching plastic parts to cans |
-
2001
- 2001-02-22 DE DE10108456A patent/DE10108456B4/en not_active Expired - Fee Related
-
2002
- 2002-02-21 IT IT2002TO000151A patent/ITTO20020151A1/en unknown
- 2002-02-22 FR FR0202268A patent/FR2821011B1/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2433406A1 (en) * | 1978-07-27 | 1980-03-14 | Shinetsu Chemical Co | PROCESS FOR IMPROVING PVC RESIN PHONOGRAPH DISCS |
| EP0136918A2 (en) * | 1983-10-04 | 1985-04-10 | Shin-Etsu Chemical Co., Ltd. | A sheet material of a vinyl chloride-based resin having improved surface properties |
| JPH0834865A (en) * | 1994-07-25 | 1996-02-06 | Kanegafuchi Chem Ind Co Ltd | Method for improving adherence of polyimide film and polyimide film improved in adherence |
| US5861192A (en) * | 1995-08-03 | 1999-01-19 | Kanegafuchi Kagaku Kogyo Kabushiki Kaisha | Method of improving adhesive property of polyimide film and polymidefilm having improved adhesive property |
Non-Patent Citations (1)
| Title |
|---|
| PATENT ABSTRACTS OF JAPAN vol. 1996, no. 06 28 June 1996 (1996-06-28) * |
Also Published As
| Publication number | Publication date |
|---|---|
| ITTO20020151A1 (en) | 2003-08-21 |
| DE10108456A1 (en) | 2002-09-12 |
| DE10108456B4 (en) | 2004-08-26 |
| ITTO20020151A0 (en) | 2002-02-21 |
| FR2821011B1 (en) | 2005-02-25 |
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| PLFP | Fee payment |
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| ST | Notification of lapse |
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