WO1999036763A1 - Ultra-accelerated natural sunlight exposure testing - Google Patents
Ultra-accelerated natural sunlight exposure testing Download PDFInfo
- Publication number
- WO1999036763A1 WO1999036763A1 PCT/US1999/000172 US9900172W WO9936763A1 WO 1999036763 A1 WO1999036763 A1 WO 1999036763A1 US 9900172 W US9900172 W US 9900172W WO 9936763 A1 WO9936763 A1 WO 9936763A1
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- WIPO (PCT)
- Prior art keywords
- concentrated
- sunlight
- gaussian
- exposure
- reflected light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/004—Investigating resistance of materials to the weather, to corrosion, or to light to light
Definitions
- This invention relates to a process for subjecting materials to accelerated irradiance exposure factors that permit about a year's worth of representative weathering to be accumulated in a period from about 3 to about 10 days, under controlled weathering conditions that include several concurrent levels of temperature and relative humidity at very high levels of natural sunlight.
- a solar concentrator which may include a High Flux Solar Furnace (HFSF) and an Irradiance Redistribution Guide (IRG)] is used to obtain elevated levels(25-100X) of concentrated sunlight for accelerated testing of material samples.
- HFSF High Flux Solar Furnace
- IRG Irradiance Redistribution Guide
- an IRG When an IRG is used, it provides the unique capability of being able to modify (redistribute) the Gaussian-shaped beam from the HFSF into a more uniform profile on a sample exposure plane.
- U.S. Patent 4,817,447 discloses a weathering chamber using lamps and sample temperature control using cooling air. Uniform sample irradiance at accelerated levels of up to 10 suns (within the UV bandwidth) appear attainable.
- a test apparatus incorporating a mirror which rejects infrared is disclosed in U.S. Patent 4,012,954.
- convective cooling air and a conductive substrate are also incorporated.
- the air movement is not used to deliver humidity to the samples during exposure; rather, humidity is provided by floating the sample substrate in a water bath.
- the '954 patent uses artificial light sources for exposure of the samples.
- U.S. Patent 3,686,940 discloses a water-cooled cylindrical mirror which rejects infrared radiation in an ultraviolet test apparatus. In the '940 patent, natural sunlight is not used.
- U.S. Patent 4,807,247 A solar weathering device with control of sample temperature by cooling air is disclosed in U.S. Patent 4,807,247. While this patent uses natural sunlight, a sample irradiance at accelerated levels of up to only 8 suns across the complete solar spectrum is employed.
- U.S. Patent 5,138,892 discloses accelerated light fastness testing of materials with xenon lamps and sample temperature control using air flow. Sample irradiance at accelerated
- UV levels of up to 8 suns (180 W/m 2 between 300-400 ran) are attainable. This patent does not utilize natural sunlight in its testing of materials.
- U.S. Patent 5,646,358 A weather test machine using xenon lamps and sample temperature and humidity control using air flow is disclosed in U.S. Patent 5,646,358. Uniform sample irradiance at accelerated levels up to only 1-3 suns (within the UV bandwidth) are attainable. This patent does not utilize natural sunlight in its weather test machine.
- U.S. Patent 5,153,780 discloses a dish reflector and method for concentrating moderate solar flux uniformly on a target plane, said dish having stepped reflective surface characterized by a plurality of ring-line segments arranged about a common axis, each segment having a concave spherical configuration.
- This need is associated with the desirability to be able to predict the in-service lifetimes of said materials and devices from correlations derived between such realistically accelerated test results and those obtained during normal use conditions. Further, there is a need to conduct these ultra - accelerated exposure tests at irradiance exposure factors of from about 25 to 100 suns, wherein the irradiance is highly uniform. Lastly, the need to conduct these ultra-accelerated natural sunlight exposure tests of materials and devices should exclude artificial light sources which invariably introduce uncertainties regarding realistic spectral content of the irradiance stress on samples being exposed. For example, the use of artificial light leads to unrealistic degradation mechanisms and failure modes of exposed materials caused by low wavelength ( ⁇ 300nm) photons that are not present in terrestrial solar spectra.
- a general object of the invention is to provide the unique capability to carry out ultra accelerated exposure testing of materials and devices under controlled conditions that include several concurrent levels of temperature and relative humidity at very high levels of natural sunlight, thereby permitting about a year's worth of representative weathering, in terms of natural sunlight exposure, to be accumulated in from about 3 to about 10 days.
- Another object of the present invention is to provide or make use of a solar concentrator (which may include an HFSF and an IRG) to provide an elevated level of sunlight having a uniform profile on a sample exposure plane.
- a solar concentrator which may include an HFSF and an IRG
- the unique capability to redistribute the highly concentrated Gaussian-shaped beam from the HFSF to a more uniform profile on the sample exposure plane is also provided.
- a further object of the present invention is to provide ultra accelerated exposure testing of materials and devices by controlling sample temperatures and humidities and demonstrating that reciprocity relationships are obeyed (i.e., level of applied accelerated stress does not change failure/degradation mode).
- a yet further object of the present invention is to provide ultra-accelerated exposure testing of materials and devices that allows materials to be subjected to accelerated irradiance exposure factors of 25-100X to provide about a year's worth of representative weathering, in terms of natural sunlight exposure, to be accumulated in from about 3 to about 10 days.
- a still further object of the invention is to provide a method of carrying out ultra accelerated exposure testing of materials and devices utilized a sample chamber that allows control of temperature and humidity during light exposure; wherein concentrated sunlight enters the chamber through an appropriate window, which may include quartz.
- a further object yet still of the invention is to provide a method for carrying out ultra accelerated exposure testing of materials and devices utilizing a cold mirror as a filter that reflects the ultraviolet /visible (UV VIS) and transmits the near infrared (NIR) part of the solar spectrum, since the short wavelength (UV) light has been shown to be the predominant deleterious stress experienced by materials and devices during outdoor weathering.
- UV VIS ultraviolet /visible
- NIR near infrared
- Another object of the present invention is to provide a method of carrying out ultra accelerated exposure testing of materials and devices under controlled weathering conditions, wherein conductive cooling of sample materials is provided by a water cooled substrate on to which samples are placed, and convective cooling is provided by blowing moist or dry air over the top surface of the samples, to provide high or low humidity to the samples during exposure of redirected concentrated sunlight into the exposure chamber to reduce the thermal load on the samples.
- the invention is accomplished by the steps of: utilizing a solar concentrator to obtain elevated levels (25-100X) of concentrated sun light on the materials or samples being tested; converting the Gaussian-shaped beam from the solar concentrator (for example, a HFSF) into a uniform flux profile having a given diameter (preferably as extended as 10 cm diameter) in the sample exposure plane (using, for example, a unique IRG; utilizing a cold mirror to reflect deleterious ultraviolet/visible (UV/VIS) light into the sample chamber; transmitting concentrated near-infrared (NIR) radiation to minimize undesirable thermal loading of material samples; and further control of temperature and relative humidity experienced by materials samples within the exposure chamber.
- Figure la depicts apparatus showing a vertically disposed irradiance redistribution guide that provides the capability of redistributing a solar beam from the HFSF without the use of a cold mirror but requiring a hot mirror as the sample exposure chamber window.
- Figure lb depicts the invention apparatus showing a substantially horizontally disposed irradiance redistribution guide that provides the capability of redistributing the Gaussian-shaped beam from the HFSF utilizing a cold mirror to provide a spectrally selective uniform profile on a sample exposure plane.
- Figure 2 is a perspective view of the system layout of the apparatus of the invention showing the sample chamber interface, via a cold mirror, with the HFSF/IRG components.
- Figure 3 shows the sample exposure chamber detail design that allows two levels of temperature and two levels of relative humidity to be maintained during sunlight exposure for the apparatus of the invention and ability to monitor spatial and spectral uniformity of the solar beam in situ during sample exposure.
- Figure 3a shows a top view of the heating/cooling chamber with samples in place.
- Figure 3b shows a top view of the chamber with humidity chamber in place.
- Figure 3c is a side view of the heating/cooling chamber.
- Figure 3d is a side view of the humidity chamber.
- Figure 4 is a graph showing sample temperature, humidity, and flux for 5 Ox sun tests demonstrating the ability to maintain control constant levels of irradiance and various combinations of temperature and relative humidity during sample exposure.
- Figure 5a is a spectroscope system operation schematic that shows how spectral reflectance measurements can be made in-situ during experiments carried out using this invention.
- Figure 5b is a spectroscope system operation schematic that shows how the spectral and spatial irradiance can be measured in-situ during experiments carried out using this invention.
- Figure 6a is a graph showing reflectance loss for samples tested at 100X.
- Figure 6b is a graph showing reflectance loss for other samples tested at 75X.
- Figure 6c is a graph showing reflectance loss for yet other samples tested at 5 OX.
- Figure 7 shows graphs of reflectance loss for three materials as a function of light intensity exposure at T ⁇ 70°C and RH ⁇ 65%.
- Figure 8 shows a graph of the calculated versus measured reflectance loss.
- Figure 9 shows data indicative of chemical/structural changes (or lack thereof) within the bulk polymer superstrate layer of exposed mirror samples.
- Figure 10 shows a cut-away view of an advanced exposure chamber design in accordance with the invention.
- Figures 1 la, 1 lb and l ie show additional views of the embodiment of the exposure chamber design of Figure 10.
- Figure 12 shows a multi-step or multi-dish parabolic reflector used in place of a heliostat, a primary concentrator, an IRG, and a cold mirror, wherein the incident sunlight NIR segment is transmitted through the multi-dish reflector, and the UV/VIS is reflected back to the sample plane.
- Figure 13 shows a multi-step parabolic concentrator used in place of a heliostat, a primary concentrator, and an IRG, employing a cold mirror to reflect UV/VIS onto a sample plane.
- Figure 14 shows a multi-step parabolic concentrator used in place of a heliostat, a primary concentrator, and an IRG, employing a hot mirror that transmits UV/VIS onto a sample plane and reflects NIR.
- the IRG provides the unique capacity of being able to modify (redistribute) the Gaussian-shaped beam from the primary concentrator to a more uniform profile on a plane located a sufficient distance behind the IRG.
- the IRG was designed to provide a uniform concentration of up to 400X (400k W/m 2 flux at nominal solar irradiance levels) within a 10 cm diameter spot at the optimal sample plane (this means that a new IRG may also be adjusted to provide a uniform concentration of 100X over a 20 cm diameter spot, ultimately allowing a four- fold increase in the number of samples that could be exposed at this nominal intensity).
- 400X 400k W/m 2 flux at nominal solar irradiance levels
- For normal materials e.g., other than concentrator PV modules designed to take advantage of such elevated flux
- lower concentration levels are needed to provide accelerated exposure conditions without destroying the samples.
- the spatial uniformity of the incident flux was measured using a fiber-probe spectral beam characterization system. This new measurement system was also sed to monitor, in situ, optical performance of sample materials being weathered.
- FIG. 2 shows the cross-sectional system layout of the IRG 20, cold mirror 21 and sample chamber 22, wherein incident concentrated sunlight ICS is passed through the IRG and uniform sunlight US exits.
- An improved chamber was designed and fabricated that allows up to four replicate samples of about 2.2cm x 2.2cm square in size each to be exposed to the same high level of accelerated solar flux at two levels each of temperature and humidity. For example, at a given flux (e.g., 50X suns), sets of samples can be simultaneously exposed at Tlow, RHlow, Tlow, Rhhigh; Thigh, RHlow; and Thigh, RH high. This allows a four-fold increase in experimental throughput at a particular exposure flux.
- a detailed drawing of the sample exposure chamber is shown in Figure 3.
- Figure 3a is a top view of the heating/cooling chamber with samples S in place, and showing heating/cooling parts HCP.
- Figure3b is a top view of the chamber with the humidity chamber in place. During testing the samples are mechanically attached to the top surface of the heating/cooling chamber to provide good thermal contact. The humidity chamber sits atop the heating/cooling chamber.
- Figure 3c is a side view of the heating/cooling chamber, showing the pathway P for fiber optic probes and the cross section view of the heaters 23.
- Figure 3d is a side view of the humidity chamber showing the humidity ports HP and the highly transmissive quartz window 24. Demonstration of Practicality by Use of the Invention:
- the base resin of the biaxially oriented superstrate material was a polymethylmethacrylate (PMMA) film.
- PMMA polymethylmethacrylate
- the first experiment used 50 suns concentration; at this level (50kW/m 2 , corrected for optical reflectance losses of the HFSF system), one years equivalent Colorado exposure would be obtained after 40.2 hours. Similarly, one years equivalent exposure would be accumulated after 26.8 hours at 75 suns after 20.1 hours at 100 suns.
- the targeted nominal temperatures were 70 °C in the hot side and the 20 °C on the cold side.
- the targeted relative humidity on the dry side was ⁇ 10% and
- the hot temperature was maintained within the desired level.
- the cold temperature was usually within 5 ° C of the set temperature.
- the dry humidity was maintained by a constant purge of dry house air, and the humid portion of the chamber was kept within 10% of the nominal targeted level.
- Figure 4 presents a closer look at representative, real-time stress conditions.
- One minute average temperatures and flux during the 50 sun test are shown.
- the hot temperatures stay between 65 and 70°C most of the time, and the cold temperatures are near 20°C.
- the humidity is shown.
- Spectral hemispherical reflectance, p 2 ⁇ ( ⁇ ) of each sample was measured before exposure and after the experiment was completed using a Perkin Elmer Lambda-9 UV-VIS-NIR spectrometer. Reflectance of samples were also periodically measured in situ using a commerically available fiberoptic reflectance probe system (The SpectraScope System operation schematics are shown in Figure 5). Use of this device is shown schematically in the reflectance mode in Figure 5 a. The SpectraScope System was also used for in situ monitoring of the spectral irradiance incident upon the samples during exposure testing. In this case, the system was configured as shown in Figure 5b. Here, ⁇ 6-7.5cm long, stripped fibers (one each UV/VIS and VIS/NIR) were inserted up through access ports at the bottom of the sample chamber SC until their highly- polished tips were coplanar with the mirror samples being exposed to concentrated sunlight.
- Figure 6 Representative plots of spectral reflectance loss are shown in Figure 6 for three materials and three levels of light intensity.
- Figure 6a corresponds to ECP-300A material exposed at 100 suns;
- Figure 6b corresponds too ECP-305 material exposed at 75 suns, and
- Figure 6c corresponds to ECP-305+ material exposed at 50 suns, respectfully. Where applicable, results for replicate samples have been averaged.
- the spectral loss in reflectance is plotted as a function of level of sunlight exposure in Figure 7 for each material tested at the most elevated temperature and humidity conditions.
- results for replicate samples have been averaged when applicable.
- the change in reflectance was calculated after a targeted cumulative dose, associated with an equivalent one year's exposure had been accumulated. The intent was to investigate two important questions. First, can these types of materials be subjected to ultra-high levels of natural sunlight (50-100X) without introducing unrealistic failure mechanisms? Second, does a reciprocity relationship exist between the level of light intensity and time of exposure?
- Figures 7a-c provide no evidence to suggest that the level of light intensity results in any systematic proclivity for loss in reflectance. That is, exposure at 50 suns for some time, t, is equivalent to exposure at 100 suns for half that time, t/2.
- Figure 7a the effect os exposure at elevated temperature and humidity at 75 suns for 32 hours is roughly the same as that resulting from exposure at 100 suns for 26.4 hours for ECP-300A. It is the cumulative dose rather than the level of intensity (within the range 50X- 100X tested) that gives rise to reflectance loss.
- RH Relative humidity (%) and A, C, and E are parameters to be fit from the measured data, ⁇ p 2 ⁇ (400).
- B was obtained from the spectral irradiance (scaled by the concentration factor associated with each experiment) and the length of exposure time.
- Table 3 presents the values of I UV . B corresponding to the three experiments.
- the various parameters specified in Equation (1) were computed from measured values of ⁇ p. 2 ⁇ (400).
- the resulting parameter estimates for each of the three materials tested are given in Table 4.
- the calculated change in performance is presented as a function of measured changes in
- Figure 8 Here, data for all three materials are shown, along with a composite linear regression line (which has been constrained to intersect the origin to reflect physical reality that no degradation occurs until light exposure begins). Note that nearly all data points are contained within a 95% prediction interval associated with this regression (dashed lines). The equation for ⁇ p is seen to provide a good representation of the data. The computed slope of the regression line is 0.88 (compared to 1.0 for perfect agreement between measured and calculated values of reflectance loss).
- the parameter estimated for the ECP-300A /aluminum substrate construction are in close agreement with previous results for a similar material construction (ECP-300 A/paint/aluminum substrate).
- E thermal activation energy parameter
- Figure 10 is a top view of an alternative embodiment of the exposure chamber design, showing a cut-away view.
- Samples 25 are disposed so that they are separated by a chamber divider 26.
- the chamber divider is in turn separated by aan insulation divider 27.
- larger heating/cooling ports 28 are disposed below the humidity ports 29.
- baffles may be added with heating and cooling using a circulating bath with an approximate range of -20 to 100 ° C , thereby eliminating the need for individual electric cartridge heaters that give rise to non-uniform sample exposure temperatures with in a given quadrant.
- the baffles and chambers may be machined out of one solid block of aluminum and enlarged slightly. This would allow more room for thermocouple wires and insulation and also provide a better seal between chambers.
- an insulated, outside shell may be fabricated, that both chambers wold rest in. This design configuration helps keep temperatures constant and makes the assembly solid.
- Figure 1 la is a top view of Figure 10 minus the samples.
- Figure 1 lb is a view taken along line A- A of Figure 11a, showing the quartz cover plate 30, the humidity chamber 31 , the insulation 32, a heating/cooling chamber with baffles 33, fiber optic guides 34, and an insulated box 35, around the chambers.
- the cold mirror fabricated for the invention system was compromised of a front surface UV reflective coating (capable of reflecting between 290-350 nm and being transparent to higher wavelength light) and a second surface visible light reflector (capable of reflecting between 350- 650 nm and transparent to light with ⁇ >650 nm). These coatings were deposited onto either side of a 3.4mm thick boro float glass substrate
- pressurized dry air typically 60 psi
- Cold mirror temperatures greater than 200 °C were reached at 100 suns.
- Concerns regarding possible shattering of the expensive cold mirror caused by thermal gradients within the plate, were further exacerbated by the possibility of thermal excursions due to transient cloud cover (in which the sun emerging from behind a cloud could momentarily deliver much higher concentration levels before the control system could react). Therefore, to provide greater cooling capacity a Vortex tube may be incorporated (a device that produces both hot and cold air from any pressurized air source) into the system design to allow cooling both sides of the mirror.
- the invention may also be accomplished by the use of a multi-step parabolic reflector 60 as depicted in Figure 12.
- the use of the multi-step dish eliminates the need for a multi- component system (heliostat, dish, IRG, cold mirror, etc.).
- a multi-step parabolic dish may be utilized, and the invention may be accomplished without the use of an irradiance guide and a cold mirror as the NIR transmitted segment NT of the incident sunlight IS is transmitted through the multi-dish reflector, and the concentrated UV/VIS flux 61 is reflected back to the sample plane 62.
- Broad band solar reflector materials can be used in conjunction with the multi-step design, thereby eliminating the need for large areas of costly spectrally selective cold mirrors located at the surface of the parabolic dish structure.
- multi-step parabolic concentrator 80 shown in Figure 14 would be to place a hot mirror, HM, so as to intercept the concentrated sunlight and transmit the UV/VIS portion of the spectrum, 81, into a sample exposure chamber located at SP, while reflecting the NIR part of the spectrum, RN.
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Abstract
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Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU23102/99A AU733241B2 (en) | 1998-01-13 | 1999-01-13 | Ultra-accelerated natural sunlight exposure testing |
EP99902977A EP1055110A4 (en) | 1998-01-13 | 1999-01-13 | Ultra-accelerated natural sunlight exposure testing |
AU2001238405A AU2001238405B2 (en) | 1998-01-13 | 2001-02-13 | Ultra-accelerated natural sunlight exposure testing facilities |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/006,746 | 1998-01-13 | ||
US09/006,746 US6073500A (en) | 1998-01-13 | 1998-01-13 | Ultra-accelerated natural sunlight exposure testing |
Publications (1)
Publication Number | Publication Date |
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WO1999036763A1 true WO1999036763A1 (en) | 1999-07-22 |
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ID=21722370
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/US1999/000172 WO1999036763A1 (en) | 1998-01-13 | 1999-01-13 | Ultra-accelerated natural sunlight exposure testing |
Country Status (4)
Country | Link |
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US (1) | US6073500A (en) |
EP (1) | EP1055110A4 (en) |
AU (1) | AU733241B2 (en) |
WO (1) | WO1999036763A1 (en) |
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WO2001067069A2 (en) * | 2000-03-09 | 2001-09-13 | Midwest Research Institute | Ultra-accelerated natural sunlight exposure testing facilities |
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WO2015112143A1 (en) * | 2014-01-23 | 2015-07-30 | Sabic Global Technologies B.V. | Method for accelerated degradation of thermoplastics |
US9557218B2 (en) | 2013-01-23 | 2017-01-31 | Sabic Global Technologies B.V. | Method for determining degradation of thermoplastics |
EP2437086A4 (en) * | 2009-05-29 | 2017-08-09 | Kuraray Co., Ltd. | Fresnel lens sheet for solar collection and design method therefor |
US9897551B2 (en) | 2013-01-23 | 2018-02-20 | Sabic Global Technologies B.V. | Method for accelerated degradation of thermoplastics |
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- 1999-01-13 EP EP99902977A patent/EP1055110A4/en not_active Ceased
- 1999-01-13 WO PCT/US1999/000172 patent/WO1999036763A1/en active IP Right Grant
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WO2001067069A3 (en) * | 2000-03-09 | 2002-02-21 | Midwest Research Inst | Ultra-accelerated natural sunlight exposure testing facilities |
EP2437086A4 (en) * | 2009-05-29 | 2017-08-09 | Kuraray Co., Ltd. | Fresnel lens sheet for solar collection and design method therefor |
EP2671066A1 (en) * | 2011-02-01 | 2013-12-11 | U.S. Coatings IP Co., LLC | Accelerated uv irradiation test on coatings |
US9557218B2 (en) | 2013-01-23 | 2017-01-31 | Sabic Global Technologies B.V. | Method for determining degradation of thermoplastics |
US9897551B2 (en) | 2013-01-23 | 2018-02-20 | Sabic Global Technologies B.V. | Method for accelerated degradation of thermoplastics |
US9921145B2 (en) | 2013-01-23 | 2018-03-20 | Sabic Global Technologies B.V. | Method for determining degradation of thermoplastics |
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KR20160098331A (en) * | 2014-01-23 | 2016-08-18 | 사빅 글로벌 테크놀러지스 비.브이. | Method for accelerated degradation of thermoplastics |
KR101944855B1 (en) | 2014-01-23 | 2019-02-01 | 사빅 글로벌 테크놀러지스 비.브이. | Method for accelerated degradation of thermoplastics |
Also Published As
Publication number | Publication date |
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AU733241B2 (en) | 2001-05-10 |
AU2310299A (en) | 1999-08-02 |
EP1055110A1 (en) | 2000-11-29 |
EP1055110A4 (en) | 2002-05-02 |
US6073500A (en) | 2000-06-13 |
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