EP1044289B1 - Boruration au plasma - Google Patents

Boruration au plasma Download PDF

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Publication number
EP1044289B1
EP1044289B1 EP98965249A EP98965249A EP1044289B1 EP 1044289 B1 EP1044289 B1 EP 1044289B1 EP 98965249 A EP98965249 A EP 98965249A EP 98965249 A EP98965249 A EP 98965249A EP 1044289 B1 EP1044289 B1 EP 1044289B1
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EP
European Patent Office
Prior art keywords
boron
vol
medium
plasma
excited
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Expired - Lifetime
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EP98965249A
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German (de)
English (en)
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EP1044289A2 (fr
Inventor
Cabeo Emilio Rodriguez
Günther LAUDIEN
Kyong-Tschong Rie
Swen Biemer
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Volkswagen AG
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Volkswagen AG
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Priority to EP01110904A priority Critical patent/EP1143031A3/fr
Publication of EP1044289A2 publication Critical patent/EP1044289A2/fr
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
    • C23C8/38—Treatment of ferrous surfaces
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding

Definitions

  • the present invention relates to a method for producing a boride layer a surface by plasma working, using a reactor Gas medium containing boron donor feeds and in the reactor Glow discharge generated.
  • US 3,677,799 A describes a method for the deposition of boron on a substrate using a gas mixture of hydrogen and a boron compound.
  • a pulsed high-frequency voltage is used, by means of which a first Hydrogen plasma is generated, which is then mixed with a boron compound to deposit a boron layer on the substrate.
  • FR 2 708 624 A1 describes a method for plasma-assisted CVD deposition of carbon layers or silicon carbide layers described using of gas mixtures, which also contain a volume percentage of gaseous boron compounds can optionally contain. This process is primarily about deposition a carbon-containing layer on a substrate. Determining the amount of one stimulated boron medium product in the glow discharge is not provided.
  • the object of the present invention is a method of the beginning mentioned genus to create the reliable to pore-free borated surfaces leads and is therefore suitable for an industrial series application.
  • the method according to the invention in its various alternatives described in more detail. Extensive tests have shown that it in plasma processing essential on the selection of the parameters of the generation of the arrives at the treatment room of the reactor. It was surprisingly found that these parameters should advantageously be selected such that an increased proportion of excited boron particles in the plasma is obtained. Contains that Plasma larger proportions of excited boron, this leads to low-pore layers. This was able to develop the method according to the invention for example by optical emission spectroscopy or plasma analysis be detected. In contrast, are BCI particles with high excitation in the plasma Containing content, then this leads to pore-rich layers resulting from those already above reasons mentioned should be avoided.
  • the inventors were able to Research has found that various parameters regarding both Generation of the plasma as well as with regard to the individual components in the contained in the gas medium to be supplied, the desired content of can influence excited boron particles. It is important that certain Thresholds of excited boron in plasma can be reached to the desired level to achieve a low-pore layer.
  • the glow discharge preferably with a pulsed DC voltage.
  • the duty cycle is defined as the ratio between the time length of the voltage pulse to the subsequent pulse pause the desired generation of an increased content of excited boron particles and thus controlling the process for plasma generation in the desired sense allows.
  • this should Duty cycle can be greater than 1.1, preferably it is in the range between about 1.25: 1 to 5: 1, more preferably in the range between 1.5: 1 and 3.5: 1.
  • the period is also d. H. the sum of the duration of the Voltage pulse and the pulse pause at below about 230 ⁇ s and in particular ⁇ 50 ⁇ s.
  • the period duration is more preferably in the method according to the invention according to a variant below about 230 ⁇ s and above 50 ⁇ s, e.g. B. at about 210 ⁇ s.
  • the applied for the pulsed direct current to generate the glow discharge is preferably in the range between about 500 volts and about 1000 volts, preferably in the range between about 600 volts and about 900 volts, more preferably in the range between about 650 volts and about 800 volts. It was also found that when working with a higher voltage, the use of a longer pulse pause is advantageous. It but can also be preferably within the achieve a good result in the above-mentioned voltage ranges, with here also the Composition of the individual components of the reactor Gas medium can exert an influence.
  • first component of the gas medium fed to the reactor is a boron donor medium Form of a boron trihalide, e.g. B. boron trichloride or boron trifluoride.
  • a boron trihalide e.g. B. boron trichloride or boron trifluoride.
  • gaseous hydrogen e.g. B. boron trichloride or boron trifluoride
  • a noble gas is used as the third component of the gas medium, z. B. Argon. It was found that when argon is used as the third component, too even when using lower voltages within the scope of the invention Good boride layers can be produced.
  • the content of boron trihalide as boron donor medium in the supplied gas medium usually affects the results of the method according to the invention.
  • the salary of boron trihalide must not be too low and should generally not be below 1 vol .-%, since then usually no suitable boride layer is obtained.
  • Boron trihalide content in the range from about 2% by volume to 50% by volume, with at However, it should be noted that high levels are relatively high Boron trihalide loss. This boron trihalide loss is found in the exhaust gas from the Reactor again and thus also leads to an increased effort in disposal or cleaning the exhaust gas.
  • the setting of the desired parameters to achieve the desired effect can one z. B. make so that the proportion of excited boron particles in the plasma determined analytically and then one or more of the process parameters for generation glow discharge such as voltage, duty cycle, frequency, temperature, pressure etc. changed accordingly.
  • the generation of Make boride layer in several stages, z. B. in a first stage works at a lower treatment temperature, thereby also for the Pore formation to avoid responsible halide formation in plasma.
  • the first stage of the process is then first of all a thinner one closed boride layer that is more resistant to corrosive attack.
  • you can then in a second treatment stage Raise the treatment temperature, thereby the diffusion of the boron particles and thus the Favor formation of a layer with increasing layer thickness.
  • the treatment temperature changes, it should be noted that also the choice of the other process parameters has to be made in such a way that a possible increased content of excited boron particles is obtained in the plasma Favor boride formation reaction and avoid a corrosive attack.
  • the current which can be set via the plasma generally has a significant influence in the context of the method according to the invention.
  • the influencing of the layer characteristics or the suppression of pore formation, caused by the chlorine species present in the treatment atmosphere, and the favoring of the boride formation, as two competing reactions, are determined via this and the other plasma parameters.
  • a plasma state can be achieved via a defined voltage, which is characterized by a high particle density of boron-releasing species, so that the boride formation takes place preferentially.
  • the analysis of the plasma states can be carried out, for example, using optical emission spectroscopy.
  • the signals for the excited boron, the excited BCI and the Cl + signal can be used to optimize the layer characteristics.
  • Procedures in which the analysis methods show high B signals have proven to be favorable. This is possible, for example, with voltages in a medium range of preferably about 650 volts to 800 volts, the content of boron trihalide in the gas medium and the pulse duty factor of the pulsed direct current also playing a role.
  • the method according to the invention is suitable for industrial applications and could be developed for series production. Compared to other known boriding processes of the type mentioned at the outset, which work with solid boron dispensing media, plasma working with a gaseous boron dispensing medium shows enormous potential for improvement.
  • the handling of the components to be treated could be reduced to a minimum.
  • the method according to the invention is suitable for automation. By changing the treatment time, a change in the gas composition is possible within the scope of the method according to the invention, so that the layer formation can be influenced thereby, special attention being paid to avoiding the formation of FeB. Furthermore, the method according to the invention takes account of the environmental concept, since the boroning agent residues to be disposed of can be minimized.
  • Industrial areas of application for the method according to the invention are e.g. B. Boronizing of metal parts to increase the wear resistance of the surfaces of components, which are subject to particularly high abrasive or adhesive loads.
  • the procedure according to the invention is suitable for. B. for use on components in the automotive industry for example for gears, hydraulic tappets, camshafts, oil pump drives z. B. with crossed axes, helical gears, continue for extruder screws and others Components that are exposed to increased stress.
  • FIG. 1 shows a diagram of the Plant structure of a plant as used in the method according to the invention Production of a boride layer on a surface can be used by plasma working is.
  • the system comprises a reactor 10 with a treatment room 11 in which the Plasma is generated.
  • the treatment room 11 of the reactor 10 is loaded with a boron donor medium, which via a gas inlet 12 and the supply line 13 in the Treatment room 11 arrives.
  • these components are Boron trihalide, e.g. B.
  • the second component is Hydrogen gas, which is supplied via the branch line 15, which is also in the Feed line 13 opens out.
  • the third component is an inert gas, e.g. B. argon that over the branch line 16 is fed, which also opens into the feed line 13.
  • mass flow meters 17, 18 and 19 by means of which the flow of the respective component of the treatment gas is adjustable and measurable.
  • the reactor 10 further comprises a charging plate 20 which is located in the reactor space 11 located and rests on two support insulators and the live support (not ) Shown.
  • the supply of voltage for generating the glow discharge takes place via the voltage supply line 21 shown schematically
  • Plasma generator delivers a pulsed DC voltage with a variable Pulse width or pulse pause as will be explained further below.
  • the composition and the flow of the treatment gas are determined using the Mass flow meters 17, 18, 19 set.
  • the measurement of the treatment pressure takes place via a gas meter independent pressure gauge and is also computer-controlled.
  • the pressure measurement and pressure control is carried out using the in the scheme with 22 designated device, the line 23 with the Treatment room 11 is connected.
  • the pressure control 22 is connected to this line 23 connected downstream a vacuum pump 24.
  • This vacuum pump 24 downstream of this device is a device 25 for Exhaust gas cleaning, which ensures adequate exhaust gas treatment.
  • the temperature of the plasma generator is regulated via the Temperature control device 26 and the line 27.
  • the system according to the invention also has an additional heater 28 which in Reactor 10 is housed to achieve the desired treatment temperature in the Treatment room 11.
  • the method according to the invention for producing a boride layer works preferably in the low pressure range, e.g. B. in the range of 1 to 10 hPa, and is by supports an electrical activation of the gas atmosphere.
  • the ones to be treated (Boronizing) components are cathodically against the container wall of the Treatment room switched.
  • the treatment temperature depends on that too boronizing material of the respective components and is, for example, above 700 ° C, preferably at 800 ° C or above.
  • a pulsed DC voltage is preferably applied in order to enable the surface to be activated by the noble gas ion bombardment before the treatment phase.
  • active excited boron particles are generated during the treatment, which reach the surface of the component and form borides there primarily by diffusion.
  • the reduction of the halogen present in the atmosphere, which is generated from the boron trihalide, is favored by the atomic hydrogen generated in the plasma, which is produced from the H 2 gas supplied.
  • the diagram according to FIG. 2 shows an example of a possible voltage curve in FIG Dependence on the time for a pulsed direct current as it is for a
  • the inventive method is particularly advantageous.
  • the voltage is z. B. in a middle range at 650 volts, the voltage pulse for example 160 microseconds is maintained and the pulse pause is, for example, 50 microseconds.
  • the pulse pause is thus about a factor of 3 shorter than the duration of the DC voltage pulse.
  • the Period duration in the exemplary embodiment is 210 microseconds and thus is Frequency 4.762 kHz.
  • the duty cycle is defined as the ratio of the length of the
  • the pulse duration for the pulse pause within a pulse is included in the exemplary embodiment 3.2. It has been found that using a relatively high voltage longer pulse pause required. When using argon in the treatment gas, but also at relatively low voltages, e.g. B. good in the range above 500 volts Get results.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Chemical Vapour Deposition (AREA)
  • Plasma Technology (AREA)
  • Electron Sources, Ion Sources (AREA)
  • Primary Cells (AREA)
  • Apparatus For Radiation Diagnosis (AREA)

Claims (17)

  1. Procédé de fabrication d'une couche de borure sur une surface utilisant la boruration au plasma, selon lequel on conduit à une zone de traitement d'un réacteur un milieu gazeux contenant un milieu source de bore et on produit dans le réacteur une décharge lumineuse, caractérisé en ce que, dans la décharge lumineuse, on détermine la quantité d'au moins un produit excité du milieu source de bore, et qu'on choisit les paramètres de fabrication du plasma produit dans la zone de traitement (11) du réacteur (10), de sorte qu'une quantité minimale et/ ou maximale du ou des différents produits excités déterminés du milieu distributeur de bore et/ ou qu'une valeur minimale et/ ou maximale d'une relation avec un ou plusieurs produits excités déterminés du milieu source de bore soit maintenue.
  2. Procédé selon la revendication 1, caractérisé en ce que, pour produire la décharge lumineuse, on utilise une tension constante pulsée avec un rapport entre la durée de la pulsion de tension et la pause de pulsion suivante supérieur à 1,1.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que, pour produire la décharge lumineuse, on utilise une tension constante avec une durée de période inférieure à 230 µs.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce qu'on travaille tout d'abord, au cours d'une première étape, à une température de traitement faible, pour éviter la formation de pores responsables de la formation d'halogénure dans le plasma et qu'on produit tout d'abord une couche de bore fine, en particulier fermée et qu'enfin, on travaille lors d'une seconde étape de traitement, à une température de traitement élevée.
  5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que la quantité du milieu excité source de bore est au moins déterminée de façon relative.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que la quantité de milieu excité source de bore est déterminée de façon spectroscopique.
  7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que du bore excité soit au moins déterminé en tant que produit du milieu excité source de bore.
  8. Procédé selon la revendication 7, caractérisé en ce que, pour former une valeur minimale et/ ou maximale, la quantité déterminée de milieu excité source de bore est mise en relation avec une quantité déterminée d'au moins un autre produit du milieu source de bore.
  9. Procédé selon l'une quelconque des revendications 1 à 8, caractérisé en ce qu'on utilise un milieu gazeux qui contient en tant que milieu source de bore, un trihalogénure de bore dans une proportion supérieure à environ 1 % en volume et parallèlement, de l'hydrogène ainsi que, le cas échéant, un gaz rare.
  10. Procédé selon l'une quelconque des revendications 1 à 9, caractérisé en ce que, pour produire le plasma, on utilise une tension constante pulsée avec un rapport entre la durée de la pulsion de tension et la pause de pulsion suivante compris entre environ 1,1:1 et 5:1, de préférence compris entre environ 1,5:1 et 3,5:1.
  11. Procédé selon l'une quelconque des revendications 1 à 10, caractérisé en ce que, pour produire le plasma, on utilise une tension constante pulsée avec une durée de période inférieure à environ 210 µs.
  12. Procédé selon l'une quelconque des revendications 1 à 11, caractérisé en ce que la durée de période est ≥ 50 µs.
  13. Procédé selon l'une quelconque des revendications 1 à 12, caractérisé en ce que, pour produire la décharge lumineuse, on utilise une tension constante pulsée comprise entre environ 500 volts et environ 1000 volts, de préférence comprise entre environ 650 volts et environ 800 volts.
  14. Procédé selon l'une quelconque des revendications 1 à 13, caractérisé en ce qu'on travaille dans une gamme de basses pressions comprise entre environ 0,5 et 15 hPa, de préférence comprise entre environ 1 et environ 10 hPa.
  15. Procédé selon l'une quelconque des revendications 1 à 14, caractérisé en ce qu'on utilise un milieu gazeux qui contient un trihalogénure de bore ayant une teneur comprise entre 2 % en volume et environ 50 % en volume, de préférence une teneur comprise entre environ 2 % en volume et environ 10 % en volume.
  16. Procédé selon l'une quelconque des revendications 1 à 15, caractérisé en ce qu'on utilise un milieu gazeux qui contient jusqu'à 20 % en volume d'un gaz rare, de préférence de l'argon, de 2 % en volume à 50 % en volume de trihalogénure de bore, de préférence de 2 % en volume à 10 % en volume de trihalogénure de bore et en outre, de l'hydrogène.
  17. Procédé selon l'une quelconque des revendications 1 à 16, caractérisé en ce qu'on utilise comme milieu distributeur de bore le BCl3 ou BF3.
EP98965249A 1997-12-15 1998-12-11 Boruration au plasma Expired - Lifetime EP1044289B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP01110904A EP1143031A3 (fr) 1997-12-15 1998-12-11 Boruration au plasma

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19755595 1997-12-15
DE19755595 1997-12-15
PCT/EP1998/008079 WO1999031291A2 (fr) 1997-12-15 1998-12-11 Boruration au plasma

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EP01110904.8 Division-Into 2001-05-05

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EP1044289B1 true EP1044289B1 (fr) 2002-03-27

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US (1) US6783794B1 (fr)
EP (2) EP1044289B1 (fr)
JP (1) JP4588213B2 (fr)
KR (1) KR100583262B1 (fr)
CN (1) CN1198953C (fr)
AT (1) ATE215132T1 (fr)
DE (1) DE59803574D1 (fr)
WO (1) WO1999031291A2 (fr)

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WO1999031291A3 (fr) 1999-09-10
EP1143031A3 (fr) 2004-04-28
JP4588213B2 (ja) 2010-11-24
WO1999031291A2 (fr) 1999-06-24
EP1044289A2 (fr) 2000-10-18
KR100583262B1 (ko) 2006-05-25
ATE215132T1 (de) 2002-04-15
US6783794B1 (en) 2004-08-31
KR20010033075A (ko) 2001-04-25
CN1282383A (zh) 2001-01-31
CN1198953C (zh) 2005-04-27
DE59803574D1 (de) 2002-05-02
EP1143031A2 (fr) 2001-10-10
JP2002508448A (ja) 2002-03-19

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