WO1999010160A1 - Method and device for hot-forming thermoplastics - Google Patents

Method and device for hot-forming thermoplastics Download PDF

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Publication number
WO1999010160A1
WO1999010160A1 PCT/EP1998/005266 EP9805266W WO9910160A1 WO 1999010160 A1 WO1999010160 A1 WO 1999010160A1 EP 9805266 W EP9805266 W EP 9805266W WO 9910160 A1 WO9910160 A1 WO 9910160A1
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WO
WIPO (PCT)
Prior art keywords
blank
radiation
radiation source
intensity
tool
Prior art date
Application number
PCT/EP1998/005266
Other languages
German (de)
French (fr)
Inventor
Kai K. O. BÄR
Rainer Gaus
Original Assignee
Industrieservis Gesellschaft Für Innovation, Technologie-Transfer Und Consulting Für Thermische Prozessanlagen Mbh
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 Industrieservis Gesellschaft Für Innovation, Technologie-Transfer Und Consulting Für Thermische Prozessanlagen Mbh filed Critical Industrieservis Gesellschaft Für Innovation, Technologie-Transfer Und Consulting Für Thermische Prozessanlagen Mbh
Priority to CA002301053A priority Critical patent/CA2301053A1/en
Priority to EP98947440A priority patent/EP1005412A1/en
Priority to AU94359/98A priority patent/AU9435998A/en
Priority to BR9811610-0A priority patent/BR9811610A/en
Priority to JP2000507520A priority patent/JP4562284B2/en
Publication of WO1999010160A1 publication Critical patent/WO1999010160A1/en

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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
    • B29C51/00—Shaping by thermoforming, i.e. shaping sheets or sheet like preforms after heating, e.g. shaping sheets in matched moulds or by deep-drawing; Apparatus therefor
    • B29C51/26—Component parts, details or accessories; Auxiliary operations
    • B29C51/42—Heating or cooling
    • B29C51/421—Heating or cooling of preforms, specially adapted for thermoforming
    • B29C51/422—Heating or cooling of preforms, specially adapted for thermoforming to produce a temperature differential
    • 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
    • B29C35/0288—Controlling heating or curing of polymers during moulding, e.g. by measuring temperatures or properties of the polymer and regulating the process
    • 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
    • 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
    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/42—Component parts, details or accessories; Auxiliary operations
    • B29C49/64—Heating or cooling preforms, parisons or blown articles
    • B29C49/6409—Thermal conditioning of preforms
    • B29C49/6418—Heating of preforms
    • 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
    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/42—Component parts, details or accessories; Auxiliary operations
    • B29C49/64—Heating or cooling preforms, parisons or blown articles
    • B29C49/6409—Thermal conditioning of preforms
    • B29C49/6436—Thermal conditioning of preforms characterised by temperature differential
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/0033—Heating devices using lamps
    • H05B3/0038—Heating devices using lamps for industrial applications
    • H05B3/0057—Heating devices using lamps for industrial applications for plastic handling and 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
    • 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
    • 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
    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/42—Component parts, details or accessories; Auxiliary operations
    • B29C49/78—Measuring, controlling or regulating

Definitions

  • the invention relates to a method and a device for thermoforming thermoplastics according to the preamble of claim 1 and the preamble of claim 12.
  • the blank has a temperature profile suitable for deformation, which is adapted to the end product to be produced.
  • a temperature profile can be relatively complicated or very inhomogeneous over the circumferential surface of the molded body.
  • an almost constant temperature over the entire wall thickness, ie the "depth" of the blank is desired.
  • hot air sources or infrared radiators in many cases also using heated molds working in several stages (e.g. in deep drawing) have been used up to now.
  • the heat can be supplied practically exclusively via the surface of the blank, so that in order to achieve the constant temperature inside the material, that is to say via its wall thickness, it is dependent on the heat transport by heat conduction within the material. This in turn presupposes a relatively slow warming up or dwell times within which the temperature compensation (over the depth of the material) can take place.
  • the method and device of the type mentioned in the introduction are complex and prone to failure.
  • the setting of a suitable temperature profile over the spatial dimensions of the blank is extremely difficult.
  • the invention has for its object to develop methods and apparatus of the type mentioned in such a way that simplified heating of the blank can be achieved with improved temperature accuracy.
  • An essential point of the invention is that the heat is supplied to the blank via radiation of a defined intensity of a radiation source in such a way that the energy is absorbed not only on the outer surfaces of the blank but also simultaneously inside the material for increasing the temperature. This in turn occurs because the intensity maximum of the radiation source is adapted to the absorption or transmission properties of the thermoplastic to be processed in such a way that the energy can actually penetrate into the material and not - as with the otherwise longer wavelengths - already in near-surface areas of the blank is absorbed.
  • the intensity maximum is preferably in the near infrared, in particular 0.8-1.4 ⁇ m, preferably 0.8-1.0 ⁇ m, ie in a range of wavelengths that are considerably shorter than the wavelengths at which the intensity maximum is more common Sources of heat radiation. It is preferred not only to achieve a considerably more uniform heating of the blank in its depth, but also a significantly faster heating. When using a temperature radiator with at least essentially a continuous radiation spectrum, this results from the fact that with the setting of the intensity maximum to shorter wavelengths proposed here, the radiation intensity increases approximately with the 4th power of the temperature of the radiator.
  • the radiation is preferably distributed to the blank by means of optical devices, in particular mirrors, gratings or similar devices of the radiation optics, such that a temperature profile adapted to the shaping device is set within the blank after the defined period of time has elapsed. So it is not the radiation source z. B. adjusted or changed by the supply of energy, rather the radiation supplied to the blank is "adjusted” according to the requirements. It is advantageous here that the radiation has its maximum intensity at the aforementioned wavelength ranges, so that the usual means of radiation optics can be used.
  • the objects or blanks to be heated are particularly preferably subjected to a radiation flux density of more than 0.5 MW / m 2 , in particular more than 1 MW / m 2 .
  • the wavelength of the intensity maximum is preferably determined by adjustment, but in particular by regulation (ie
  • Measurement and feedback of the relevant radiation quantities) of the temperature of a heating element The setting of the filament temperature of a halogen lamp is particularly preferred. Since this has to be set to relatively high temperatures (which are unusually high for halogen lamps (in order to achieve the short wavelengths mentioned)), appropriate measures are preferably taken to nevertheless ensure a long service life of the halogen lamp used. In particular, special cooling measures are taken both in the area of the (quartz) glass bodies and in the area of the base of the halogen lamps.
  • the distance between the radiation source and the blank and / or an optical filter device such as grating or gray filter or the like and / or chopper devices is preferably used alternatively or cumulatively.
  • the procedure is preferably such that the defined heating or irradiation period does not significantly exceed 10 seconds, particularly preferably 5 seconds. This ensures, on the one hand, that the usual blanks or preforms are evenly heated, and on the other hand, production can be carried out at high speed.
  • the preform is preferably handed over to the molding tool, in particular a blow-stretching device, for deformation essentially immediately after exposure to the radiation without a substantial dwell time free of radiation exposure. This ensures that the temperature profile set (in particular by optics) along the body cannot change due to heat conduction within the preform.
  • the blank is deformed from the tool onto the blank in an essentially cold tool without substantial heat input.
  • this can be done by molding the blank in a single drawing operation. This ensures that the temperature profile set (in particular by optical means) in the blank is essentially maintained and the risk of the blank sticking to the deep-drawing tool is avoided, as is the case in particular with those deep-drawing tools in which the heating of the blank is done by the tool itself.
  • the device according to the invention thus comprises a radiation source with a regulating device for regulating an emission wavelength range of the radiation source in such a way that the intensity maximum of the radiation source lies in a wavelength range within which the thermoplastic has a low degree of absorption or a higher degree of transmission than incident or incident light at longer wavelengths Radiation absorbs or lets through or lets in.
  • This radiation source is preferably designed so that its in- intensity maximum in the near infrared, in particular 0.8 to 1.4 and particularly preferably 0.8 to 1.0 ⁇ m.
  • the degree of absorption should be so low or the degree of transmission so high that a penetration depth of the radiation corresponding to the thickness of the blank to be processed is ensured and the blank is not only on its surface but from the beginning (i.e. without temperature compensation via heat conduction) is heated inside.
  • Mirrors, gratings or similar devices of the radiation optics are preferably provided in order to heat the blank with a temperature profile which is optimal for shaping.
  • a current controller is preferably provided for regulating the filament temperature, which current value is obtained from a correspondingly designed sensor (pyrometer) in order to determine the filament temperature or the wavelength range, at which the intensity maximum of the radiation source is to be kept constant and adjusted according to the specifications mentioned at the beginning.
  • the intensity is controlled (by applying disturbance variables or by comparing target and actual values) so that the desired temperature profile is reached within the set time of exposure to radiation.
  • This intensity setting can be done by the distance between the radiation source and the blank and / or optical filter devices and / or a chopper device, which so to speak "radiation packets" get to the blank, the chopper speed being chosen so that the "packet durations" are very short in relation to the Total period over which energy is supplied to the blank.
  • the arrangement is selected in such a way that the blank can be produced within a period of less than 10 sec, preferably from less than 5 sec in the area of the radiation source and removed from it again, so that no substantial temperature compensation can occur while changing the temperature profile (set by optical devices).
  • the entire device for the production of PET bottles is designed and equipped with stations located close to one another (radiation source, molding tool) and with fast conveying devices, so that there is no significant dwell time of the blank or preform within which radiation energy is applied can be done for heating before deformation in the blow-stretching device. This also keeps the set temperature profile in the preform.
  • a deep-drawing tool In the production of deep-drawn parts, a deep-drawing tool is used which has a relatively low temperature (measured in relation to the deep-drawing tools previously used), preferably only a single deep-drawing tool being provided, and the blank being thus formed in a single deep-drawing process.
  • the advantage here is that there is no significant change in the temperature profile previously set by the corresponding radiation energy supply.

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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Toxicology (AREA)
  • Blow-Moulding Or Thermoforming Of Plastics Or The Like (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

According to the inventive method for hot-forming thermoplastics, a blank, preform or similar semi-finished product is heated to a preforming temperature and then deformed using a forming device. Said blank is subjected to radiation of a set intensity for a set period of time. The maximum intensity of the source of said radiation lies in an emission wavelength range in which the thermoplastic absorbs the radiation emitted at a lower absorption ratio than for longer wavelengths. The invention also relates to a device for hot-forming thermoplastics, comprising a heat supply device for heating the blank, preform or similar semi-finished product to a preforming temperature, and a forming device, especially a blow-(stretch)-device, a deep draw device or similar forming tool for deforming the heated blank. Said heating device comprises a radiation source which is provided with a regulating device for regulating an emission spectrum to ensure that the maximum intensity of said radiation source lies in an emission wavelength range in which the thermoplastic absorbs the radiation emitted at a lower absorption ratio than for longer wavelengths.

Description

Verfahren und Vorrichtung zum Warmverformen von Thermoplasten Method and device for thermoforming thermoplastics
Beschreibungdescription
Die Erfindung betrifft ein Verfahren und eine Vorrichtung zum Warmverformen von Thermoplasten nach dem Oberbegriff des Patentanspruches 1 bzw. dem Oberbegriff des Patentanspruches 12.The invention relates to a method and a device for thermoforming thermoplastics according to the preamble of claim 1 and the preamble of claim 12.
Bei derartigen Verfahren bzw. Vorrichtungen kommt es ganz wesentlich darauf an, daß der Rohling ein zur Verformung geeignetes Temperaturprofil aufweist, das dem herzustellenden Endprodukt angepaßt ist. Ein derartiges Temperaturprofil kann bei komplizierten Formen des Produktes, insbesondere dann, wenn niedrige Wandstärken gewünscht sind, relativ kompliziert bzw. über die Umfangsflache des Formkörpers hinweg sehr inhomogen seien. Gewünscht ist allerdings eine nahezu konstante Temperatur über die gesamte Wandstärke, also die "Tiefe" des Rohlings. Um dies zu erreichen, wird bisher insbesondere mit Heißluftquellen oder auch Infrarotstrahlern, in vielen Fällen auch mit beheizten, in mehreren Stufen arbeitenden Formen (z. B. beim Tiefziehen) gearbeitet. Hierbei kann die Wärme praktisch ausschließlich über die Oberfläche des Rohlings zugeführt werden, so daß man zur Erzielung der konstanten Temperatur im Materialinneren, also über dessen Wandstärke auf den Wärmetransport durch Wärmeleitung innerhalb des Materials angewiesen ist. Dies wiederum setzt eine relativ langsame Erwärmung bzw. Verweilzeiten voraus, innerhalb derer der Temperaturausgleich (über die Tiefe des Materials) stattfinden kann. Dadurch werden Verfahren und Vorrichtung der eingangs genannten Art aufwendig und störanfällig. Insbesondere ist auch die Einstellung eines geeigneten Temperaturprofils über die räumlichen Ausdehnungen des Rohlings ausgesprochen schwierig.In such methods and devices, it is very important that the blank has a temperature profile suitable for deformation, which is adapted to the end product to be produced. In the case of complicated shapes of the product, in particular when low wall thicknesses are desired, such a temperature profile can be relatively complicated or very inhomogeneous over the circumferential surface of the molded body. However, an almost constant temperature over the entire wall thickness, ie the "depth" of the blank, is desired. In order to achieve this, hot air sources or infrared radiators, in many cases also using heated molds working in several stages (e.g. in deep drawing) have been used up to now. In this case, the heat can be supplied practically exclusively via the surface of the blank, so that in order to achieve the constant temperature inside the material, that is to say via its wall thickness, it is dependent on the heat transport by heat conduction within the material. This in turn presupposes a relatively slow warming up or dwell times within which the temperature compensation (over the depth of the material) can take place. As a result, the method and device of the type mentioned in the introduction are complex and prone to failure. In particular, the setting of a suitable temperature profile over the spatial dimensions of the blank is extremely difficult.
Der Erfindung liegt die Aufgabe zugrunde, Verfahren und Vorrichtung der eingangs genannten Art dahingehend weiterzubilden, daß eine vereinfachte Erwärmung des Rohlings mit verbesserter Temperatur-Genauigkeit erzielbar ist.The invention has for its object to develop methods and apparatus of the type mentioned in such a way that simplified heating of the blank can be achieved with improved temperature accuracy.
Diese Aufgabe wird durch ein Verfahren nach Anspruch 1 bzw. eine Vorrichtung nach Anspruch 12 gelöst.This object is achieved by a method according to claim 1 and an apparatus according to claim 12.
Ein wesentlicher Punkt der Erfindung liegt darin, daß die Wärme über Strahlung definierter Intensität einer Strahlungsquelle dem Rohling so zugeführt wird, daß die Energie nicht nur an den Außenflächen des Rohlings sondern auch gleichzeitig im Inneren des Materials zur Temperaturerhöhung aufgenommen wird. Dies wiederum geschieht dadurch, daß das Intensitätsmaximum der Strahlungsquelle derart auf die Absorptions- bzw. Trans- missionseigenschaften des zu bearbeitenden Thermoplasten angepaßt wird, daß die Energie auch tatsächlich in das Material eindringen kann und nicht - wie bei den sonst üblichen längeren Wellenlängen - schon in oberflächennahen Bereichen des Rohlings absorbiert wird.An essential point of the invention is that the heat is supplied to the blank via radiation of a defined intensity of a radiation source in such a way that the energy is absorbed not only on the outer surfaces of the blank but also simultaneously inside the material for increasing the temperature. This in turn occurs because the intensity maximum of the radiation source is adapted to the absorption or transmission properties of the thermoplastic to be processed in such a way that the energy can actually penetrate into the material and not - as with the otherwise longer wavelengths - already in near-surface areas of the blank is absorbed.
Vorzugsweise liegt das Intenstitätsmaximum im nahen Infrarot, insbesondere bei 0,8 - 1,4 μm, vorzugsweise bei 0,8 - 1,0 μm, also in einem Bereich von Wellenlängen, die erheblich kürzer sind als die Wellenlängen, bei welchen das Intensitätsmaximum üblicher Wärmestrahlungsquellen liegt. Bevorzugtermaßen wird nicht nur eine erheblich gleichmäßigere Erwärmung des Rohlings in seiner Tiefe erreicht, sondern auch eine erheblich schnellere Erwärmung. Bei Verwendung eines Temperaturstrahlers mit zumindest im wesentlichen einem kontinuierlichen Strah- lungsspektrum ergibt sich dies dadurch, daß bei der hier vorgeschlagenen Einstellung des Intensitätsmaximums auf kürzere Wellenlängen die Strahlungsintensität etwa mit der 4. Potenz der Temperatur des Strahlers zunimmt. Vorzugsweise wird die Strahlung mittels optischer Einrichtungen, insbesondere Spiegel, Gitter oder dergleichen Einrichtungen der Strahlungs-Optik derart verteilt dem Rohling zugeführt, daß ein der Formeinrichtung angepaßtes Temperaturprofil innerhalb des Rohlings nach Ablauf des definierten Zeitraums eingestellt wird. Es wird also nicht die Strahlungsquelle z. B. durch Energiezufuhr eingestellt bzw. verändert, es wird vielmehr die dem Rohling zugeführte Strahlung den Anforderungen entsprechend "eingestellt". Hierbei ist es von Vorteil, daß die Strahlung ihr Intensitätsmaximum bei den vorgenannten Wellenlängenbereichen aufweist, so daß die üblichen Mittel der Strahlungs-Optik verwendbar sind.The intensity maximum is preferably in the near infrared, in particular 0.8-1.4 μm, preferably 0.8-1.0 μm, ie in a range of wavelengths that are considerably shorter than the wavelengths at which the intensity maximum is more common Sources of heat radiation. It is preferred not only to achieve a considerably more uniform heating of the blank in its depth, but also a significantly faster heating. When using a temperature radiator with at least essentially a continuous radiation spectrum, this results from the fact that with the setting of the intensity maximum to shorter wavelengths proposed here, the radiation intensity increases approximately with the 4th power of the temperature of the radiator. The radiation is preferably distributed to the blank by means of optical devices, in particular mirrors, gratings or similar devices of the radiation optics, such that a temperature profile adapted to the shaping device is set within the blank after the defined period of time has elapsed. So it is not the radiation source z. B. adjusted or changed by the supply of energy, rather the radiation supplied to the blank is "adjusted" according to the requirements. It is advantageous here that the radiation has its maximum intensity at the aforementioned wavelength ranges, so that the usual means of radiation optics can be used.
Besonders vorzugsweise werden die zu erwärmenden Objekte bzw. Rohlinge mit einer Strahlungsflußdicht über 0,5 MW/m2, insbesondere über 1 MW/m2 beaufschlagt.The objects or blanks to be heated are particularly preferably subjected to a radiation flux density of more than 0.5 MW / m 2 , in particular more than 1 MW / m 2 .
Vorzugsweise wird die Wellenlänge des Intensitätsmaximums durch Einstellung, insbesondere aber durch eine Regelung (alsoThe wavelength of the intensity maximum is preferably determined by adjustment, but in particular by regulation (ie
Messung und Rückführung der relevanten Strahlungsgrößen) der Temperatur eines Heizelements eingestellt. Besonders bevorzugt ist hierbei die Einstellung der Wendel-Temperatur einer Halogenlampe. Nachdem diese auf relativ hohe, für Halogenlampen un- üblich hohe Temperaturen (zur Erreichung der genannten kurzen Wellenlängen) eingestellt werden muß, sind vorzugsweise entsprechende Maßnahmen getroffen, um dennoch eine lange Lebensdauer der verwendeten Halogenlampe zu gewährleisten. Insbesondere werden hierfür besondere Kühlungsmaßnahmen sowohl im Be- reich der (Quarz- )Glaskörper als auch im Bereich der Sockel der Halogenlampen getroffen.Measurement and feedback of the relevant radiation quantities) of the temperature of a heating element. The setting of the filament temperature of a halogen lamp is particularly preferred. Since this has to be set to relatively high temperatures (which are unusually high for halogen lamps (in order to achieve the short wavelengths mentioned)), appropriate measures are preferably taken to nevertheless ensure a long service life of the halogen lamp used. In particular, special cooling measures are taken both in the area of the (quartz) glass bodies and in the area of the base of the halogen lamps.
Um nun die Intensität den Anforderungen entsprechen einzustellen, wird vorzugsweise alternativ oder kumulativ die Ent- fernung zwischen der Strahlungsquelle und dem Rohling und/oder eine optische Filtereinrichtung wie Gitter oder Graufilter oder dergleichen und/oder Choppereinrichtungen verwendet. Bei dem kommerziell besonders interessanten Bereich der Verwendung des Verfahrens zur Herstellung von Polyethylen-Flaschen wird vorzugsweise so vorgegangen, daß der definierte Aufheizoder Bestrahlungs-Zeitraum 10 sec, besonders bevorzugterweise 5 sec nicht wesentlich überschreitet. Dadurch ist zum einen eine gleichmäßige Erwärmung der üblichen Rohlinge oder Preforms sichergestellt, andererseits kann mit hoher Geschwindigkeit produziert werden.In order to adjust the intensity to the requirements, the distance between the radiation source and the blank and / or an optical filter device such as grating or gray filter or the like and / or chopper devices is preferably used alternatively or cumulatively. In the commercially interesting area of use of the process for the production of polyethylene bottles, the procedure is preferably such that the defined heating or irradiation period does not significantly exceed 10 seconds, particularly preferably 5 seconds. This ensures, on the one hand, that the usual blanks or preforms are evenly heated, and on the other hand, production can be carried out at high speed.
Der Preform wird vorzugsweise im wesentlichen unmittelbar nach Beaufschlagung mit der Strahlung ohne wesentliche strahlungsbe- aufschlagungsfreie Verweildauer dem Formwerkzeug, insbesondere einer Blas-Streck-Einrichtung zur Verformung übergeben. Dadurch ist sichergestellt, daß sich das (insbesondere durch Optiken) eingestellte Temperaturprofil entlang des Körper nicht durch Wärmeleitung innerhalb des Preforms verändern kann.The preform is preferably handed over to the molding tool, in particular a blow-stretching device, for deformation essentially immediately after exposure to the radiation without a substantial dwell time free of radiation exposure. This ensures that the temperature profile set (in particular by optics) along the body cannot change due to heat conduction within the preform.
Zur Herstellung von Tiefziehteilen ist es bevorzugt, wenn der Rohling in einem, im wesentlichen kalten Werkzeug ohne wesent- liehe Wärmezufuhr von dem Werkzeug auf den Rohling verformt wird. Insbesondere kann dies geschehen, indem der Rohling in einem einzigen Ziehvorgang geformt wird. Dadurch ist gewährleistet, daß das (insbesondere durch optische Mittel) eingestellte Temperatur-Profil im Rohling im wesentlichen beibehal- ten bleibt und die Gefahr eines Anklebens des Rohlings am Tiefziehwerkzeug vermieden wird, wie dies insbesondere bei solchen Tiefziehwerkzeugen der Fall ist, bei welchen die Erwärmung des Rohlings durch das Werkzeug selbst erfolgt.For the production of deep-drawn parts, it is preferred if the blank is deformed from the tool onto the blank in an essentially cold tool without substantial heat input. In particular, this can be done by molding the blank in a single drawing operation. This ensures that the temperature profile set (in particular by optical means) in the blank is essentially maintained and the risk of the blank sticking to the deep-drawing tool is avoided, as is the case in particular with those deep-drawing tools in which the heating of the blank is done by the tool itself.
Die erfindungsgemäße Vorrichtung umfaßt also eine Strahlungsquelle mit einer Regeleinrichtung zum Regeln eines Emissionswellenlängenbereichs der Strahlungsquelle derart, daß das Intensitätsmaximum der Strahlungsquelle in einem Wellenlängenbereich liegt, innerhalb dessen der Thermoplast mit einem niedri- gen Absorptionsgrad bzw. einem höheren Transmissionsgrad als bei längeren Wellenlängen einfallende oder auftreffende Strahlung absorbiert bzw. hindurchläßt oder eindringen läßt. Diese Strahlungsquelle ist vorzugsweise so ausgebildet, daß ihr In- tensitätsmaximum im nahen Infrarot, insbesondere bei 0,8 bis 1,4 und besonders bevorzugterweise bei 0,8 bis 1 , 0 μm liegt. Der Absorptionsgrad soll hierbei so niedrig sein bzw. der Transmissionsgrad so hoch sein, daß eine der Dicke des zu bear- beitenden Rohlings entsprechende Eindringtiefe der Strahlung sichergestellt ist und der Rohling nicht nur an seiner Oberfläche sondern von Anfang an (also ohne Temperaturausgleich über Wärmeleitung) in seinem Inneren erwärmt wird.The device according to the invention thus comprises a radiation source with a regulating device for regulating an emission wavelength range of the radiation source in such a way that the intensity maximum of the radiation source lies in a wavelength range within which the thermoplastic has a low degree of absorption or a higher degree of transmission than incident or incident light at longer wavelengths Radiation absorbs or lets through or lets in. This radiation source is preferably designed so that its in- intensity maximum in the near infrared, in particular 0.8 to 1.4 and particularly preferably 0.8 to 1.0 μm. The degree of absorption should be so low or the degree of transmission so high that a penetration depth of the radiation corresponding to the thickness of the blank to be processed is ensured and the blank is not only on its surface but from the beginning (i.e. without temperature compensation via heat conduction) is heated inside.
Vorzugsweise werden Spiegel, Gitter oder dergleichen Einrichtungen der Strahlungs-Optik vorgesehen, um den Rohling mit einem Temperaturprofil zu erwärmen, welches zur Formung optimal ist.Mirrors, gratings or similar devices of the radiation optics are preferably provided in order to heat the blank with a temperature profile which is optimal for shaping.
Bei der als Strahlungsquelle vorzugsweise vorgesehenen Halogenlampe oder dergleichen Strahlungseinrichtung mit einem Heizelement ist vorzugsweise zur Regelung der Wendel-Temperatur ein Stromregler vorgesehen, der einen Ist-Wert aus einem entsprechend ausgebildeten Fühler (Pyrometer) erhält, um die Wendel- temperatur bzw. den Wellenlängenbereich, bei welchem sich das Intensitätsmaximum der Strahlungsquelle befindet, konstant zu halten und entsprechend den eingangs genannten Vorgaben einzustellen.In the case of the halogen lamp or similar radiation device with a heating element, which is preferably provided as the radiation source, a current controller is preferably provided for regulating the filament temperature, which current value is obtained from a correspondingly designed sensor (pyrometer) in order to determine the filament temperature or the wavelength range, at which the intensity maximum of the radiation source is to be kept constant and adjusted according to the specifications mentioned at the beginning.
Weiterhin wird auch die Intensität (durch StörgrößenaufSchaltung bzw. einen Vergleich von Soll- und Ist-Werten) geregelt, so daß innerhalb der eingestellten Zeit der Strahlungsbeaufschlagung das gewünschte Temperaturprofil erreicht wird. Diese Intensitätseinstellung kann durch die Entfernung zwischen Strahlungsquelle und Rohling und/oder optische Filtereinrichtungen und/oder eine Choppereinrichtung geschehen, welche sozusagen "Strahlungspakete" zum Rohling gelangen lassen, wobei die Choppergeschwindigkeit so gewählt ist, daß die "Paketdauern" sehr kurz sind in Relation zum Gesamtzeitraum, über welchen dem Rohling Energie zugeführt wird.Furthermore, the intensity is controlled (by applying disturbance variables or by comparing target and actual values) so that the desired temperature profile is reached within the set time of exposure to radiation. This intensity setting can be done by the distance between the radiation source and the blank and / or optical filter devices and / or a chopper device, which so to speak "radiation packets" get to the blank, the chopper speed being chosen so that the "packet durations" are very short in relation to the Total period over which energy is supplied to the blank.
Bei der Herstellung von PET-Flaschen wird die Anordnung derart gewählt, daß der Rohling innerhalb einer Zeitdauer von unter 10 sec, vorzugsweise von unter 5 sec in den Bereich der Strahlungsquelle gebracht und aus diesem wieder entfernt wird, so daß kein wesentlicher Temperaturausgleich unter Abänderung des (durch optische Einrichtungen) eingestellten Temperaturprofils geschehen kann. Zusätzlich oder auch alternativ wird die gesamte Vorrichtung zur Herstellung von PET-Flaschen derart ausgebildet und mit nahe beieinander liegenden Stationen (Strahlungsquelle, Formwerkzeug) und mit schnellen Fördereinrichtungen ausgestattet, daß keine wesentliche Verweildauer des Rohlings bzw. Preforms vorliegt, innerhalb deren eine Beaufschlagung mit Strahlungsenergie zur Erwärmung vor der Verformung in der Blas-Streck-Einrichtung geschehen kann. Auch dadurch wird das eingestellte Temperaturprofil im Preform erhalten.In the production of PET bottles, the arrangement is selected in such a way that the blank can be produced within a period of less than 10 sec, preferably from less than 5 sec in the area of the radiation source and removed from it again, so that no substantial temperature compensation can occur while changing the temperature profile (set by optical devices). Additionally or alternatively, the entire device for the production of PET bottles is designed and equipped with stations located close to one another (radiation source, molding tool) and with fast conveying devices, so that there is no significant dwell time of the blank or preform within which radiation energy is applied can be done for heating before deformation in the blow-stretching device. This also keeps the set temperature profile in the preform.
Bei der Herstellung von Tiefziehteilen wird ein Tiefziehwerk- zeug benutzt, welches eine relativ (gemessen an den bisher benutzten Tiefziehwerkzeugen) niedrige Temperatur aufweist, wobei vorzugsweise lediglich ein einziges Tiefziehwerkzeug vorgesehen ist und damit der Rohling in einem einzigen Tiefziehvorgang geformt wird. Auch hierbei liegt der Vorteil wieder darin, daß keine wesentliche Veränderung des zuvor durch die entsprechende Strahlungsenergie-Zufuhr eingestellten Temperaturprofils erfolgt. In the production of deep-drawn parts, a deep-drawing tool is used which has a relatively low temperature (measured in relation to the deep-drawing tools previously used), preferably only a single deep-drawing tool being provided, and the blank being thus formed in a single deep-drawing process. Again, the advantage here is that there is no significant change in the temperature profile previously set by the corresponding radiation energy supply.

Claims

Verfahren und Vorrichtung zum Warmverformen von ThermoplastenPatentansprüche Method and device for thermoforming thermoplastics
1. Verfahren zum Warmverformen von Thermoplasten, wobei ein Rohling, Preform oder dergleichen Halbzeug auf eine Ver- formungstemperatur aufgewärmt und durch eine Formeinrichtung, insbesondere eine Blas (-Streck)Einrichtung, eine Tiefzieheinrichtung oder dergleichen Formwerkzeug verformt wird, d a d u r c h g e k e n n z e i c h n e t, daß der Rohling während eines definierten Zeitraums mit einer Strahlung definierter Intensität einer Strahlungsquelle beaufschlagt wird, die ein Intensitätsmaximum in einem Emissionswellenlängenbereich aufweist, innerhalb dessen der Thermoplast mit einem niedrigeren Absorptionsgrad Strahlung absorbiert bzw. mit einem höheren1. A method for thermoforming thermoplastics, wherein a blank, preform or the like semi-finished product is heated to a shaping temperature and deformed by a shaping device, in particular a blowing (stretching) device, a deep-drawing device or the like molding tool, characterized in that the blank during a defined period of time is subjected to radiation of a defined intensity from a radiation source which has an intensity maximum in an emission wavelength range, within which the thermoplastic absorbs radiation with a lower degree of absorption or with a higher one
Transmissionsgrad strahlungsdurchlässig ist als bei längeren Wellenlängen.Transmittance is translucent than at longer wavelengths.
2. Verfahren nach Anspruch 1, d a d u r c h g e k e n n z e i c h n e t, daß das Intensitätsmaximum im nahen Infrarot liegt.2. The method of claim 1, d a d u r c h g e k e n n z e i c h n e t that the intensity maximum is in the near infrared.
3. Verfahren nach Anspruch 2, d a d u r c h g e k e n n z e i c h n e t, daß das Intensitätsmaximum bei 0,8 - 1,4 μm Wellenlänge, vorzugsweise bei 0,8 - 1,0 μm Wellenlänge liegt. 3. The method according to claim 2, characterized in that the maximum intensity at 0.8 - 1.4 microns wavelength, preferably at 0.8 - 1.0 microns wavelength.
4. Verfahren nach Anspruch 1, d a d u r c h g e k e n n z e i c h n e t, daß das Intensitätsmaximum in einem Wellenlängenbereich, in welchem der Thermoplast ein Absorptionsband aufweist, dessen Absorptionsgrad 75%, vorzugsweise 50% nicht übersteigt.4. The method of claim 1, d a d u r c h g e k e n n z e i c h n e t that the intensity maximum in a wavelength range in which the thermoplastic has an absorption band, the degree of absorption does not exceed 75%, preferably 50%.
5. Verfahren nach einem der vorhergehenden Ansprüche, d a d u r c h g e k e n n z e i c h n e t, daß die Strahlung mittels optischer Einrichtungen, insbesondere Spiegel, Gitter oder dergleichen Einrichtungen der Strahlung-Optik derart verteilt dem Rohling zugeführt wird, daß ein der Formeinrichtung angepaßtes Temperaturprofil innerhalb des Rohlings nach Ablauf des definierten Zeitraums eingestellt wird.5. The method according to any one of the preceding claims, characterized in that the radiation is supplied to the blank by means of optical devices, in particular mirrors, gratings or similar devices of the radiation optics, such that a temperature profile adapted to the shaping device within the blank after the defined period has expired is set.
6. Verfahren nach einem der vorhergehenden Ansprüche, d a d u r c h g e k e n n z e i c h n e t, daß die Wellenlänge des Intensitätsmaximums durch Einstellung, insbesondere durch Regelung der Temperatur eines Heizelementes, insbesondere einer Wendel einer Halogenlampe eingestellt wird.6. The method according to any one of the preceding claims, that the wavelength of the intensity maximum is adjusted by setting, in particular by regulating the temperature of a heating element, in particular a filament of a halogen lamp.
7. Verfahren nach einem der vorhergehenden Ansprüche, d a d u r c h g e k e n n z e i c h n e t, daß die Intensität durch Einstellung, insbesondere durch Regelung einer Entfernung zwischen der Strahlungsquelle und dem Rohling und/oder eine optische Filtereinrichtung wie Gitter und/oder Graufilter und/oder durch Choppereinrich- tung eingestellt wird.7. The method according to any one of the preceding claims, that the intensity is adjusted by setting, in particular by regulating a distance between the radiation source and the blank and / or an optical filter device such as grating and / or gray filter and / or by chopper device.
8. Verfahren nach einem der vorhergehenden Ansprüche zur Herstellung von PET-Flaschen, d a d u r c h g e k e n n z e i c h n e t, daß der definierte Zeitraum 10 sec, vorzugsweise 5 sec nicht wesentlich überschreitet. 8. The method according to any one of the preceding claims for the production of PET bottles, characterized in that the defined period does not significantly exceed 10 seconds, preferably 5 seconds.
. Verfahren nach Anspruch 8, d a d u r c h g e k e n n z e i c h n e t, daß der Preform im wesentlichen unmittelbar nach der Beaufschlagung mit der Strahlung ohne wesentliche strahlungsbe- aufschlagungsfreie Verweildauer im Formwerkzeug, insbesondere in einer Blas-Streck-Einrichtung verformt wird.. A method according to claim 8, and that the preform is deformed substantially immediately after exposure to the radiation without a substantial dwell time in the molding tool, in particular in a blow-stretching device.
10. Verfahren nach einem der vorhergehenden Ansprüche zur Herstellung von Tiefziehteilen, d a d u r c h g e k e n n z e i c h n e t, daß der Rohling mit einem, im wesentlichen kalten Werkzeug ohne wesentliche Wärmezufuhr von dem Werkzeug auf den Rohling verformt wird.10. The method according to any one of the preceding claims for the production of deep-drawn parts, d a d u r c h g e k e n n z e i c h n e t that the blank is deformed from the tool to the blank with a substantially cold tool without substantial heat supply.
11. Verfahren nach Anspruch 10, d a d u r c h g e k e n n z e i c h n e t, daß der Rohling in einem einzigen Ziehvorgang geformt wird.11. The method according to claim 10, d a d u r c h g e k e n n z e i c h n e t that the blank is formed in a single drawing.
12. Vorrichtung zum Warmverformen von Thermoplasten, umfassend eine Wärmezuführeinrichtung, zum Erwärmen eines Rohlings, Preform oder dergleichen Halbzeug auf eine Verformungstemperatur und eine Formeinrichtung, insbesondere eine Blas(-Streck)Einrichtung, eine Tiefzieheinrichtung oder dergleichen Formwerkzeug zum Verformen des aufgewärmten Rohlings, d a d u r c h g e k e n n z e i c h n e t, daß die Erwärmungseinrichtung eine Strahlungsquelle umfaßt, die mit einer Regeleinrichtung zum Regeln eines Emissions- Spektrums der Strahlungsquelle derart ausgestattet ist, daß ein Intensitätsmaximum der Strahlungsquelle in einem Emissionswellenlängenbereich liegt, innerhalb dessen der Thermoplast mit einem niedrigen Absorptionsgrad bzw. einem höheren Transmissionsgrad als bei längeren Wellenlängen einfallende oder auftreffende Strahlung absorbiert bzw. hindurchläßt. 12. Apparatus for thermoforming thermoplastics, comprising a heat supply device, for heating a blank, preform or the like semi-finished product to a shaping temperature and a shaping device, in particular a blowing (stretching) device, a deep-drawing device or the like shaping tool for shaping the warmed blank, characterized in that that the heating device comprises a radiation source which is equipped with a control device for regulating an emission spectrum of the radiation source such that an intensity maximum of the radiation source lies in an emission wavelength range within which the thermoplastic has a lower degree of absorption or a higher degree of transmission than at longer wavelengths absorbing or transmitting incident or incident radiation.
13. Vorrichtung nach Anspruch 12, d a d u r c h g e k e n n z e i c h n e t, daß die Strahlungsquelle derart ausgebildet ist und geregelt wird, daß ihr Intensitätsmaximum im nahen Infrarot liegt.13. The apparatus of claim 12, d a d u r c h g e k e n n z e i c h n e t that the radiation source is designed and controlled so that its intensity maximum is in the near infrared.
14. Vorrichtung nach Anspruch 13, d a d u r c h g e k e n n z e i c h n e t, daß die Strahlungsquelle derart ausgebildet ist und geregelt wird, daß ihr Intensitätsmaximum bei 0,8 - 1,4 μm, vor- zugsweise bei 0,8 - 1,0 μm liegt.14. The device according to claim 13, so that the radiation source is designed and controlled in such a way that its intensity maximum is 0.8-1.4 μm, preferably 0.8-1.0 μm.
15. Vorrichtung nach Anspruch 12, d a d u r c h g e k e n n z e i c h n e t, daß die Strahlungsquelle derart ausgebildet ist und geregelt wird, daß ihr Intensitätsmaximum in einem Wellenlängenbereich liegt, in welchem der Thermoplast ein Absorptionsband aufweist, dessen Absorptionsgrad 75%, vorzugsweise 50% nicht übersteigt.15. The apparatus of claim 12, d a d u r c h g e k e n n z e i c h n e t that the radiation source is designed and controlled such that its intensity maximum is in a wavelength range in which the thermoplastic has an absorption band whose degree of absorption does not exceed 75%, preferably 50%.
16. Vorrichtung nach einem der Ansprüche 12 bis 15, d a d u r c h g e k e n n z e i c h n e t, daß die Strahlungsquelle eine Halogenlampe oder dergleichen Strahlungseinrichtung mit einem Heizelement umfaßt, und daß die Regelung einen Stromregler zur Einstellung und Re- gelung der Temperatur der Strahlungseinrichtung, insbesondere einer Wendel der Halogenlampe umfaßt.16. Device according to one of claims 12 to 15, that the radiation source comprises a halogen lamp or similar radiation device with a heating element, and that the control comprises a current regulator for setting and regulating the temperature of the radiation device, in particular a filament of the halogen lamp.
17. Vorrichtung nach einem der Ansprüche 12 bis 16, g e k e n n z e i c h n e t durch eine Intensitätsregelungseinrichtung zur Regelung der17. Device according to one of claims 12 to 16, g e k e n e z e i c h n e t by an intensity control device for controlling the
Intensität der dem Rohling zugeführten Energie, umfassend eine Entfernungs-Einstelleinrichtung zum Einstellen einer Entfernung zwischen der Strahlungsquelle und dem Rohling und/oder eine optische Filtereinrichtung wie Gitter oder Graufilter und/oder Choppereinrichtungen. Intensity of the energy supplied to the blank, comprising a distance setting device for setting a distance between the radiation source and the blank and / or an optical filter device such as grating or gray filter and / or chopper devices.
18. Vorrichtung nach Anspruch 12 zur Herstellung von PET-Fla- schen, g e k e n n z e i c h n e t durch eine Zeiteinstelleinrichtung, die derart ausgebildet ist, daß dem Rohling eine Strahlung definierter Intensität über einen definierten Zeitraum zuführbar ist, der 10 sec, vorzugsweise 5 sec nicht wesentlich überschreitet.18. Apparatus according to claim 12 for the production of PET bottles, g e k e n n e e e c h n e t by a time setting device which is designed such that radiation of a defined intensity can be supplied to the blank over a defined period of time which does not substantially exceed 10 sec, preferably 5 sec.
19. Vorrichtung nach Anspruch 12 zur Herstellung von PET-Fla- sehen, d a d u r c h g e k e n n z e i c h n e t, daß die Strahlungsquelle innerhalb einer im wesentlichen kontinuierlich arbeitenden Produktionsstraße im wesentlichen derart unmittelbar vor der Formeinrichtung angebracht ist, daß der Preform im wesentlichen unmittelbar nach der Beaufschlagung mit der Strahlung ohne wesentliche strah- lungsbeaufschlagungsfreie Verweildauer im Formwerkzeug, insbesondere in einer Blas-Streck-Einrichtung verformt wird.19. The device according to claim 12 for the production of PET fla see, characterized in that the radiation source is mounted within an essentially continuously working production line substantially in such a way immediately in front of the molding device that the preform essentially immediately after exposure to the radiation without significant dwell time in the molding tool, particularly in a blow-stretching device, is deformed without exposure to radiation.
20. Vorrichtung nach einem der Ansprüche 12 bis 17 zur Herstellung von Tiefziehteilen, d a d u r c h g e k e n n z e i c h n e t, daß die Formeinrichtung im wesentlichen unbeheizt derart aus- gebildet ist, daß der Rohling mit einem, im wesentlichen kalten Werkzeug ohne wesentliche Wärmezufuhr zur Temperaturerhöhung des Rohlings verformbar ist.20. Device according to one of claims 12 to 17 for the production of deep-drawn parts, d a d u r c h g e k e n z e i c h n e t that the molding device is designed essentially unheated such that the blank can be deformed with a substantially cold tool without substantial heat supply to increase the temperature of the blank.
21. Vorrichtung nach Anspruch 20, d a d u r c h g e k e n n z e i c h n e t, daß ein einziges Tief zieh-Werkzeug vorgesehen ist. 21. The apparatus of claim 20, d a d u r c h g e k e n n z e i c h n e t that a single deep-drawing tool is provided.
PCT/EP1998/005266 1997-08-21 1998-08-19 Method and device for hot-forming thermoplastics WO1999010160A1 (en)

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AU94359/98A AU9435998A (en) 1997-08-21 1998-08-19 Method and device for hot-forming thermoplastics
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DE19736462C2 (en) 2003-06-18
EP1005412A1 (en) 2000-06-07
DE19736462A1 (en) 1999-02-25
CN1267253A (en) 2000-09-20
CA2301053A1 (en) 1999-03-04
JP2001513465A (en) 2001-09-04
BR9811610A (en) 2000-09-05
JP4562284B2 (en) 2010-10-13
AU9435998A (en) 1999-03-16

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