EP1015401B1 - Method of forming flares having igniters formed from extrudable igniter compositions - Google Patents

Method of forming flares having igniters formed from extrudable igniter compositions Download PDF

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Publication number
EP1015401B1
EP1015401B1 EP98936941A EP98936941A EP1015401B1 EP 1015401 B1 EP1015401 B1 EP 1015401B1 EP 98936941 A EP98936941 A EP 98936941A EP 98936941 A EP98936941 A EP 98936941A EP 1015401 B1 EP1015401 B1 EP 1015401B1
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EP
European Patent Office
Prior art keywords
igniter
fibers
water
weight percent
oxidizer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP98936941A
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German (de)
English (en)
French (fr)
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EP1015401A1 (en
Inventor
Daniel B. Nielson
Gary K. Lund
Reed J. Blau
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Northrop Grumman Innovation Systems LLC
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Alliant Techsystems Inc
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Publication date
Priority claimed from US09/119,518 external-priority patent/US6170399B1/en
Application filed by Alliant Techsystems Inc filed Critical Alliant Techsystems Inc
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    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
    • C06C5/00—Fuses, e.g. fuse cords
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
    • C06C9/00—Chemical contact igniters; Chemical lighters
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
    • C06C15/00—Pyrophoric compositions; Flints

Definitions

  • the present invention relates to a method of forming a flare comprising an extrudable igniter composition.
  • Igniter compositions ought to satisfy a number of design criteria.
  • the igniter composition, when formed, should be sufficiently robust to remain in operable form prior to deployment of the device to be ignited, such as a flare or other device.
  • One of the commonly proposed igniter systems uses solid particles consisting of B/KNO 3 which, when ignited, initiate combustion of the specified gas generant composition.
  • the present invention offers a method of forming flares incorporating one or more of the herein disclosed igniter sticks.
  • the extrudable igniter is readily manufactured at low cost to obtain a physically robust product.
  • the igniter can be manufactured without the use of a thermopiastic melt or hot-melt mixing equipment, and thus avoids the potential hazards associated with processing at such elevated temperatures.
  • the extrudable Igniter composition from which the igniter stick can be formed is suitably processed at ambient temperatures into robust products which have sufficiently relatively selectable ignition characteristics.
  • the igniter stick can have other configurations, provided the configuration is consistent with the objectives herein disclosed.
  • the extrudable Igniter composition can be used to form a solid. or hollow igniter "stick" capable of igniting a flare or propellant composition in a flare or other pyrotechnic device.
  • the extruded igniter sticks formed by the method of the invention can be characterized as having a configuration designed for rapid deflagration at a high temperature upon ignition.
  • an igniter stick Upon ignition an igniter stick is capable of igniting another pyrotechnic composition,
  • the igniter sticks are sized to be capable of complete end to end ignition, e.g., complete flame transition, in a short time, such as less than 10 miliseconds.
  • the igniter compositions which are capable of being extruded comprise a combination of a water-soluble binder, water-soluble or dispersable oxidizing agent, water-soluble or dispersable fuel, and a selected amount of water.
  • the extrudable compositions are essentially compositionally homogeneous.
  • the binder is a water-soluble binder, comprising at least one member selected from the group consisting of a water-soluble gum present in an amount of about 2 weight percent to about 10 weight percent based on the total amount of dry ingredients in the extrudable igniter composition, poly-N-vinyl pyrolidone, polyvinyl alcohols and copolymers thereof, polyacrylamide, sodium polyacrylates, copolymers based on acrylamide or sodium acrylate, and water-soluble gelatin.
  • These water soluble gums include naturally occurring gums, such as guar gum, acacia gum, modified celluloses and starches. A detailed discussion of "gums" is provided by C.L.
  • the suitable fuels and oxidizers can be water soluble or water insoluble. Suitable fuels and oxidizers can be inorganic or organic.
  • the binder concentration is such that a sufficiently mechanically robust extrudate is obtained.
  • the extrudate such as an igniter stick, should be capable of retaining its shape, e.g. maintaining its integrity, prior to ignition.
  • the extruded igniter stick is capable of being received (inserted) in a pyrotechnic composition, e.g. a suitably configured bore (e.g. central bore) in a propellant composition, and of shattering or fracturing when ignited.
  • the binder can be in a range of, for example, of about 2 % by weight to about 10 % by weight, and more particularly about 3% by weight to about 7% by weight, relative to the dry ingredients in the formulation.
  • the binder can be comprised of more than one binder material.
  • the igniter composition includes at least one oxidizer, which is preferably water soluble or at least water dispersable.
  • the oxidizer can therefore be organic or inorganic, although inorganic oxidizers are presently preferred.
  • Organic oxidizers which are dispersable in a binder so that a sufficiently homogeneous igniter composition is obtainable include amine nitrate salts, nitro compounds, nitramine, nitrate esters, and amine perchlorates, of which methyl ammonium nitrate, methyl ammonium perchlorate are are exemplary.
  • Other canditates include RDX and HMX, CL-20 and PETN.
  • Inorganic oxidizers include oxidizing ionic species such as nitrates, nitrites, chlorates, perchlorates, peroxides, and superoxides.
  • oxidizing ionic species such as nitrates, nitrites, chlorates, perchlorates, peroxides, and superoxides.
  • metal nitrates such as potassium nitrate or strontium nitrate, ammonium nitrate, meta
  • perchlorates such as potassium perchlorate
  • metal peroxides such as strontium peroxide.
  • the oxidizer is ordinarily present in an amount effective to ensure oxidation of at least the fuel in the igniter and can be in a range of, for example, of about 40% by weight to about 90% by weight, and more particularly about 70% by weight to about 85% by weight, rotative to the dry ingredients in the formulation.
  • the igniter composition can be formulated with an additional fuel, assuming that the binder may be capable of functioning as a secondary, not primary, fuel for the igniter composition.
  • additional fuels include powdered metals, such as powdered aluminum, zirconium, magnesium and/or titanium, among others; metal hydrides such as zirconium or titanium hydride; and so-called metalloids, such as silicon and boron which are capable of being sufficiently "dispersable" in the binder.
  • Water-soluble or water-dispersable fuels include, e.g., guanidine nitrate, cyano compounds, nitramines (RDX and/or HMX), CL-20, tetranitrocarbazoles, organic nitro compounds, and may, if desired, be "multi-modal" in particle size distribution. Water dispersable materials can be added in substantially even particle size distribution or in multi-modal distributions depending on the ignition characteristics desired.
  • Water dispersable fuels are, by present preference, used in fine particulate form, such as powder or ground to sufficient fine particles, to ensure adequate distribution during the manufacturing process. By preference, an at least substantially even distribution in the resultant extrudable igniter composition is desired.
  • the fuel is in pulverulent form, such as 100 ⁇ or less, such as, for example, from about 1 ⁇ to 30 ⁇ .
  • Metals in powder form may have, if desired, a smaller particle size range, such as from about 1 to 20 ⁇ , or even smaller such as 1 to about 5 ⁇ .
  • the amount of fuel -- other than the binder -- can be in a range of, for example, of about 5 to about 30% by weight, and more particularly about 10% by weight to about 20% by weight, rotative to the dry ingredients in the formulation.
  • the present igniter sticks and related grains can incorporate, if desired, a reinforcement.
  • Suitable reinforcement can be achieved with fibers, such as combustible fibers, which can serve to both strengthen the extruded igniter stick, and, upon appropriate selection of the reinforcement, improve igniter performance.
  • the fibers are preferably generally shorter in length (low aspect ratio).
  • Fibers incorporated into extrudable igniter formulations include, for instance, polyolefin fibers, polyamide fibers, polyester fibers and poly (2,2-(m-phenylene)-5,5-bisbenzimidazole (“PBI”) fibers.
  • Polyolefin fibers include polyethylene ("PE") fibers, such as PE fibers having an outer diameter of about 0.005 mm and higher, such as to about 0.8 mm, and a length in a range of 0.1 mm to about 3.2 mm, of which the Spectra 900 brand of polyethylene fiber from Allied-Signal is illustrative.
  • PE polyethylene
  • Suitable polyamide fibers such as Nylon 6 fibers, can have a suitably selected diameter, such as 19 microns, and a length of 1.5 mm to about 6.4 mm.
  • Suitable polyester fibers include high tenacity polyester fibers having lengths of about 1.5 mm to about 6.4 mm, and a suitable diameter of about 25 microns.
  • PBI fibers include those having lengths on the order of 0.8 mm to 3.2 mm. Representative reinforced igniter sticks and the formulations therefor are reported in the Examples.
  • composition in extrudable form for use in the method of the invention is readily obtainable, for instance, by mixing binder, fuel, oxidizer and the selected amount of water for such a period of time to achieve an at least substantially even distribution of the fuel and oxidizer throughout the binder.
  • the method involves mixing a water-soluble binder and a selected amount of water to form a pre-mix, and admixing the pre-mix with (a) first the fuel and then the oxidizer, or (b) the oxidizer and then the fuel, or (c) a combination of the oxidizer and fuel.
  • the amount of water is generally such that the resultant product has a consistency which is extrudable, but. by preference, is not runny. In principle greater amounts of water can be used but some manufacturing concerns may arise, including an increase in waste water laden with varying amounts of pyrotechnic species (fuel, oxidizer etc.).
  • the igniter composition thus formed is capable of being extruded to the desired physical geometry.
  • suitable flares are those known to those skilled in the art as thrusted flares of which the MJU-10 flare is exemplary.
  • Other flares such as M-206 flares (which may or may not be spectrally matched) or a near IR flare, such as a M-278 type flare, are also suitably combined with one or more igniter sticks.
  • the suitable flares are not restricted to the aforementioned MJU-10, M-206 or M-278 flares.
  • a so-called standard 6.99 cm (2.75 inch) (cross-section diameter) flare, including visible illuminating flares are suitably provided with at least one igniter stick.
  • Non-commercial flare variants of the standard flare such as the M-257 type flare
  • the igniter stick decreases the costs, decreases the fabrication time, and simplifies the design of flares, including the ignition system for a thrusted flare such as the MJU-10 flare.
  • Igniter sticks can be used in a great number of decoy devices which include decoy flares which are deployed to defend against an incoming threats, and particularly against heat-seeking missiles.
  • the igniter sticks improve the reliability of flare ignition by decreasing out-of-place first fire, and the safety of manufacturing flares by eliminating the use of flammable solvents commonly used when applying traditional first fires.
  • Suitable flares and/or flare compositions for combination with at least-one igniter stick are described in Encylopedia of Chemical Technology, 20 :680-697 (4th ed, 1996), including the references cited therein, the complete disclosure of which is incorporated herein by reference.
  • Figure 1 illustrates, in cross-section, a type of flare known as a XM212 flare, in the longitudinal cross section view, the casing is a suitable pressure enclosure fabricated from steel or other material capable of being used for a flare application.
  • the cartridge case 18 can have a vented housing 17.
  • the opposing end of the XM212 flare includes an aft closure 12, spacers 13, an ignition system with igniter 15, protective cap 10 and a piston 11.
  • a solidified (extruded) igniter stick 16 which may be solid or hollow, extends lengthwise (completely or partially) through the propellant grain as shown in Figure 1.
  • the igniter stick is formed by extruding the hereinabove described extrudable igniter composition, allowing the extrudate to solidify, and inserting it into the propellant grain (preferably before its cured.)
  • a selected propellant composition 14 surrounds the igniter stick.
  • a so-called rapid deflagration cord if desired, can be disposed lengthwise, e.g., such as loosely sleeved, within a hollow igniter stick.
  • more than one igniter stick can, if desired, be used.
  • FIG. 2-5 Cross sectional "diameter" views of flare casings with propellant and igniter sticks are shown in Figures 2-5.
  • the flare case 28 can, if desired, have a foam layer 22 (e.g. a foamed nitrocellulose liner) sprayed on its interior surface before propellant 24 is loaded.
  • a center bore having a pre-selected geometry 26 sleeves a hollow igniter stick 20 (in end view such as quargum binder/B/KNO 3 ).
  • the flare case 38 has been loaded with propellant 34 and provided with a centrally positioned hollow igniter stick 36.
  • additional solid or hollow igniter sticks 32 can be provided.
  • flare case 48 is loaded with propellant 44, and a centrally positioned shaped bore of pre-selected geometry.
  • the centrally positioned bore may have an igniter stick 42 with igniter sticks 46 (in strip form) disposed radially in the slots from the bore.
  • the igniter sticks are fitted within the slots, and preferably are not loosly fitted.
  • the flare case 58 is shown loaded with propellant 54 and a centrally positioned igniter stick having multiple axial bores therein.
  • the igniter stick can, if desired, be fitted with a peelable glove/sleeve prior to its insertion into the propellant grain. This can protect an igniter stick during the manufacturing process or during storage before use.
  • the igniter sticks are preferably inserted into the propellant grain before the latter is cured.
  • the igniter formulation was extruded through a 12 point star die with a maximum diameter of 0.84 cm (0.33") and a minimum diameter of 0.76 cm (0.30").
  • the die included a central 0.203 cm (0.080") diameter pin, thus producing a hollow rod-like configuration.
  • the extruded igniter formulation was cut into 17.8 cm (7") lengths.
  • a series of extruded igniter stick formulations containing boron, potassium nitrate, a water-soluble binder, and optionally, fibers for reinforcement were prepared. These formulations are reported in Table I. The formulations were first mixed on a 10 g and then a 30 g scale to determine their sensitivity towards stimuli including impact. friction, electrostatic discharge, and heat (Table II). In general, carbohydrate-based binders exhibited the greatest sensitivity with respect to ABL friction. Formulations containing methyl cellulose, guar gum, and locust bean gum as the binder were also used to prepare igniter sticks.
  • the igniter formulation was extruded through a 12 point star die with a maximum diameter of 0.84 cm (0.33") and a minimum diameter of 0.775 cm (0.305"). The die included a centrally located 0.20 cm (0.80") diameter pin.
  • the extruded igniter formulation was cut into 17.8 cm (7") lengths. Before drying, a 19.1 cm (7.5") length of 0.18 cm (0.07") diameter Teledyne RDC (rapidly deflagrating cord) was inserted. Ten additional 5.1 cm (2") lengths were extruded. The igniter sticks were dried at 74°C (165 F) overnight.
  • Leaching of a mixture of KNO 3 and binder to the surface of the grain may occur for some formulations during drying. Leaching in the perforation is not desired. Leaching was found to be least important in formulations containing tragacanth gum, Cyanamer® A-370 and Cyanamer® P-21 (Table III). igniter sticks from the formulations containing Cyanamer® A-370 and Cyanamer® P-21 were evaluated in content with an inflator device. Relative drying rates of 10 :1.7 : 1 were calculated for formulations containing Cyanamer® N-300, Cyanamer® P-21 and Cyanamer® A-370, respectively. Thus, the formulation containing Gyanamer® A-370 was shown to dry quickly, with minimal KNO 3 leaching producing a grain that ignites gas generant with minimal ignition delays.
  • a series of igniters containing fibers were formulated with the goal of enhancing durability of the extruded igniter sticks as seen from Table IV. All formulations exhibited favorable safety characteristics. Samples (325 g) of each formulation were mixed in a Baker-Perkins pint mixer with 13.5 parts/100 of water. After dry blending the KNO 3 and Cyanamer® A-370 for one minute, the water was added followed by five minutes of mixing. The fiber was then added in two increments and the boron in three increments with three minutes of mixing after each addition. After a final "scrape down", the formulation was mixed for an additional ten minutes. The resulting brown, dough-like material was granulated to -4 mesh and fed into a Haake 25 mm single-screw extruder.
  • the igniter formulation was extruded through a 12 point star die with a maximum diameter of 0.84 cm (0.33") and a minimum diameter of 0.775 cm (0.305").
  • the die included a centrally located 0.38 cm (0.15") diameter pin.
  • the extruded igniter formulation was cut into 17.8 cm (7") lengths. Ten additional 5.1 cm (2") lengths were extruded.
  • the igniter sticks were dried at 74°C (165 F) overnight.
  • the "fiber ID” can be characterized as carbon fiber, alumina fiber, aluminosilicate, polyethylene, and polybenzimidizole.
  • An extrudable igniter composition was obtained by forming a pre-mix of guar gum (5.0 wt%, 0.25 gram) and water (deionized 15.0 wt%, 1.75 grams); combining the pre-mix with potassium nitrate (average particle size of about 26 microns, 75 wt%, 3.75 grams); and adding thereto fuel, boron (amorphous; 20.0 wt%, 1.00 gram).
  • An extrudable igniter composition was obtained as in Example 4, but 20.0 wt% of water was used.
  • An extrudable igniter composition was prepared as in Example 4, except that the amount of fuel, boron, was increased to 22.0 wt% (1.10 grams) and the amount of binder, guar gum, was reduced to 3.0 wt% (0.15 gram).
  • An extrudable igniter composition was prepared according to the procedure of Example 4, except that the binder was polyacrylamide (cyanamer "N-300” from American Cyanamid, 5.0 wt%, 0.25 gram).
  • An extrudable igniter mixture is prepared by adding potassium nitrate (210 grams) and a polyacrylamide (14 gram; cyanamer "N-300" from American Cyanamid) to a bowl; adding water (44.8 grams), to the bowl and mixing for 1 minute; and adding boron (amorphous; 56.0 grams) thereto followed by mixing for about four minutes.
  • An extrudable igniter composition was prepared as in Example 8, except that the amount of water is 50.4 grams, the potassium nitrate and binder are first dry-blended together before adding the water and mixing 1 minute. The powdered boron is then added and the mixing is continued for four minutes.
  • the igniter composition prepared according to Example 8 was granulated, dried and pressed into 1.3 cm (1 ⁇ 2 inch) diameter by 2.5 cm (1 inch) long pellets. The pellets were then inhibited on all but one face and combusted in a closed pressurized vessel at 6.9 x 10 6 , 13.8 x 10 6 , and 20.7 x 10 6 N/m 2 (1000, 2000 and 3000 psi) via ignition of the uninhibited face. Burning rates of 10.6 cm/s (4.16 ips), 10.97 cm/s (4.32 ips) and 11.23 cm/s (4.42 ips) respectively, were observed.
  • a portion of the wet igniter composition prepared as described in Example 9 was placed in a 5.1 cm (2 in) diameter ram extruder and forced through an appropriate die so as to provide a center perforated cylindrical extrudate of approx 0.8 cm (0.3 in) diameter with a perforation diameter of approx 0.15 cm (0.06 in).
  • This extrudate was partially dried and cut into 17.8 cm (7 in) lengths prior to final drying.
  • the resulting igniter sticks were then tested in a gas generating device consisting of a tubular metal cylinder approx 20.3 cm (8 in) long by approx 5.1 cm (2 in) diameter dosed at both ends and provided with radial ports.
  • One of the end closures was further provided with an initiating squib.
  • the igniter stick was retained in the center of the tube and a 17.8 cm (7 in) length of rapid deflagration cord (RDC) placed in the center perforation of the stick.
  • the gas generating device was then filled with a charge of gas generant pellets and tested in a closed tank. Comparable results were obtained with the igniter stick in contrast to those obtained with a conventional ignition train in which a perforated metal tube filled with a like quantity of ignition powder and the RDC replaces the igniter stick/RDC combination. In all cases ignition of the gas generant pellets was observed to occur within 8 msec.
  • the igniter sticks were cut into 15.2 cm (6 inch) lengths and dried at 57°C (135°F) overnight prior to use.
  • the center perforated ignitor sticks were successfully demonstrated in an XM-212 decoy flare. Two XM 212 grains were fabricated. One with the traditional slurry first fire and the other with three center perforated igniter sticks.
  • a flare configuration with an igniter stick is shown in Figure 1.
  • the igniter sticks were also incorporated in the main ignition system of a MJU-10 decoy flare.
  • the MJU-10 flare requires a larger igniter than the XM-212 flare. Therefore, the igniter formulation was extruded through a 12 point star die that has a 0.84 cm (0.33 inch) maximum diameter a 0.76 cm (0.30 inch) minium diameter.
  • the extrusion die also included a 0.20 cm (0.80 inch) diameter pin used to produce a center perforated grain.
  • the extruded igniter sticks were cut to 12.7 cm (5.0 inch) lengths and then dried at 57°C (135°F) for 24 hours. The igniter sticks were then inserted into the center perforation of the MJU-10 flare grain.
  • the MJU-10 flare was successfully ignited with the igniter stick.
  • the igniter stick will decrease the cost, decrease the fabrication time, and simplify the design of an ignition system for the thrusted MJU-10 flare.
  • igniter sticks can be used in a great number of decoy flare devices. They will aid in improving the reliability of flare ignition by decreasing out-of-place first fire, and also improve the safety of manufacturing flares by eliminating the use of flammable solvents commonly used when applying traditional first fires.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Non-Portable Lighting Devices Or Systems Thereof (AREA)
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EP98936941A 1997-09-04 1998-07-22 Method of forming flares having igniters formed from extrudable igniter compositions Expired - Lifetime EP1015401B1 (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US119518 1987-11-12
US5750197P 1997-09-04 1997-09-04
US57501P 1997-09-04
US09/119,518 US6170399B1 (en) 1997-08-30 1998-07-21 Flares having igniters formed from extrudable igniter compositions
PCT/US1998/015064 WO1999011587A1 (en) 1997-09-04 1998-07-22 Flares having igniters formed from extrudable igniter compositions

Publications (2)

Publication Number Publication Date
EP1015401A1 EP1015401A1 (en) 2000-07-05
EP1015401B1 true EP1015401B1 (en) 2004-12-08

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EP98936941A Expired - Lifetime EP1015401B1 (en) 1997-09-04 1998-07-22 Method of forming flares having igniters formed from extrudable igniter compositions

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EP (1) EP1015401B1 (ko)
JP (1) JP4057779B2 (ko)
KR (1) KR100545187B1 (ko)
CN (1) CN100537492C (ko)
AU (1) AU750304B2 (ko)
BR (1) BR9812622A (ko)
CA (1) CA2302359C (ko)
DE (1) DE69828068T2 (ko)
IL (1) IL134859A (ko)
WO (1) WO1999011587A1 (ko)

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US7469640B2 (en) 2006-09-28 2008-12-30 Alliant Techsystems Inc. Flares including reactive foil for igniting a combustible grain thereof and methods of fabricating and igniting such flares

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EP2305624B1 (en) * 2009-10-01 2017-09-27 Maxamcorp Holding, S.L. Self-degradable explosive device
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CN110325814B (zh) * 2016-12-01 2022-07-22 巴泰勒纪念研究所 自发光材料、示踪弹药和照明装置
US10557696B2 (en) 2016-12-01 2020-02-11 Battelle Memorial Institute Self-glowing materials and tracer ammunition
JP7379142B2 (ja) * 2019-12-23 2023-11-14 株式会社トクヤマ 金属窒化物の製造方法、着火剤及び着火剤成形体
JP7312690B2 (ja) * 2019-12-23 2023-07-21 株式会社トクヤマ 金属窒化物の製造方法、及び着火剤成形体

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Publication number Priority date Publication date Assignee Title
US7469640B2 (en) 2006-09-28 2008-12-30 Alliant Techsystems Inc. Flares including reactive foil for igniting a combustible grain thereof and methods of fabricating and igniting such flares
US7690308B2 (en) 2006-09-28 2010-04-06 Alliant Techsystems Inc. Methods of fabricating and igniting flares including reactive foil and a combustible grain

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IL134859A (en) 2004-02-08
AU8577598A (en) 1999-03-22
EP1015401A1 (en) 2000-07-05
KR100545187B1 (ko) 2006-01-24
WO1999011587A1 (en) 1999-03-11
CA2302359C (en) 2006-10-24
AU750304B2 (en) 2002-07-18
JP2003524743A (ja) 2003-08-19
DE69828068T2 (de) 2005-04-21
DE69828068D1 (de) 2005-01-13
JP4057779B2 (ja) 2008-03-05
CN1273572A (zh) 2000-11-15
KR20010023660A (ko) 2001-03-26
CN100537492C (zh) 2009-09-09
BR9812622A (pt) 2000-08-22
CA2302359A1 (en) 1999-03-11
IL134859A0 (en) 2001-05-20

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