WO2007032862A2 - Matières générant des gaz - Google Patents

Matières générant des gaz Download PDF

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Publication number
WO2007032862A2
WO2007032862A2 PCT/US2006/032422 US2006032422W WO2007032862A2 WO 2007032862 A2 WO2007032862 A2 WO 2007032862A2 US 2006032422 W US2006032422 W US 2006032422W WO 2007032862 A2 WO2007032862 A2 WO 2007032862A2
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WO
WIPO (PCT)
Prior art keywords
gas generant
generant composition
composition
nitrate
basic
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Application number
PCT/US2006/032422
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English (en)
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WO2007032862A3 (fr
Inventor
Ivan V. Mendenhall
Robert D. Taylor
Original Assignee
Autoliv Asp, Inc.
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Publication date
Application filed by Autoliv Asp, Inc. filed Critical Autoliv Asp, Inc.
Publication of WO2007032862A2 publication Critical patent/WO2007032862A2/fr
Publication of WO2007032862A3 publication Critical patent/WO2007032862A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
    • C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
    • C06D5/06—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
    • C06B23/007—Ballistic modifiers, burning rate catalysts, burning rate depressing agents, e.g. for gas generating
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt

Definitions

  • This invention relates generally to a material for use in gas generation such as for forming an inflation gas such as for inflating inflatable devices such as airbag cushions included in automobile inflatable restraint systems.
  • Such airbag restraint systems normally include: one or more airbag cushions, housed in an uninflated and folded condition to minimize space requirements; one or more crash sensors mounted on or to the frame or body of the vehicle to detect sudden deceleration of the vehicle; an activation system electronically actuated by the crash sensors; and inflator device that produces or supplies a gas to inflate the airbag cushion.
  • the crash sensors actuate the activation system which in turn actuates the inflator device which begins to inflate the airbag cushion in a matter of milliseconds.
  • inflator devices have been disclosed in the art for inflating one or more inflatable restraint system airbag cushions.
  • such inflator devices may include one or more pyrotechnic compositions such as an igniter composition, the combustion of which may ignite a gas generating compound, or a gas generant composition, the combustion of which provides a gas such as may be used either alone or to supplement a stored and pressurized gas to inflate an associated airbag cushion.
  • Pyrotechnic gas generant compositions commonly utilized in the inflator devices of automobile inflatable restraint systems had previously most typically employed or been based on sodium azide. Such sodium azide-based compositions upon initiation normally produce or form nitrogen gas. While the use of sodium azide and certain other azide-base pyrotechnic materials meets current industry specifications, guidelines and standards, such use may involve or raise potential concerns such as involving safe and effective handling, supply and disposal of such azide-based pyrotechnic materials. As a result, the development and use of other suitable gas generant compositions has been pursued. In particular, such efforts have been directed to the development of azide-free gas generant compositions for use in such inflator devices.
  • non-azide or azide-free gas generant formulations or compositions that provide: a high gas output, typically greater than about 2 moles of gas per 100 grams of composition; a low combustion temperature such as a combustion flame temperature of less than 2000 K; a high burn rate, generally greater than about 0.85 inches per second at 3000 psi; low toxicity of effluent gases; and easily filterable particulate matter.
  • a high gas output typically greater than about 2 moles of gas per 100 grams of composition
  • a low combustion temperature such as a combustion flame temperature of less than 2000 K
  • a high burn rate generally greater than about 0.85 inches per second at 3000 psi
  • low toxicity of effluent gases and easily filterable particulate matter.
  • azide-free formulations are less toxic and therefore easier to dispose of and more readily accepted by the general public.
  • a higher burn rate than can be achieved with such pyrotechnic compositions may be desired for inflator programs requiring higher performance. Still further, it is generally desirable to increase or maximize the loading density of the gas generant or pyrotechnic and thus reduce or minimize the volume of the required associated chamber.
  • a vehicle may include a driver airbag, a passenger airbag, one or more seat belt pretensioners, one or more knee bolsters, and/or one or more inflatable belts, each with an associated inflator device, to protect the driver and passengers from frontal crashes.
  • the vehicle may also include one or more head/thorax cushions, thorax cushions, and/or curtains, each with at least one associated inflator device, to protect the driver and passengers from side impact crashes.
  • gaseous effluent or inflation gas produced by all of the inflator devices within a particular vehicle when taken as whole, are required to satisfy strict content limitations in order to meet current industry safety guidelines.
  • gas generant compositions used in such inflator devices produce as little as possible of undesirable effluents such as hydrogen chloride, carbon monoxide, ammonia, nitrogen dioxide and nitric oxide.
  • combustion flame temperature of a gas generant material typically has a significant effect on the levels of carbon monoxide and nitrogen oxides in the gas effluent. More specifically at temperatures above 2000 K, the prevalence of reactions within and between gaseous species in the effluent such as to produce carbon monoxide and nitrogen oxides can dramatically increase. In contrast at combustion flame temperatures below 2000 K, these reactions occur to a significantly lesser extent such as may desirably result in cleaner, less toxic, effluent gases.
  • a general object of the invention is to provide an improved gas generant composition.
  • a more specific objective of the invention is to overcome one or more of the problems described above.
  • the general object of the invention can be attained, at least in part, through a gas generant composition that includes a non-azide, organic, nitrogen-containing fuel; a substituted basic metal nitrate comprising a reaction product of an acidic organic compound and abasic metal nitrate; and at least one transition metal complex of diammonium bitetrazole effective to decrease the burn rate pressure sensitivity of the gas generant composition as compared to the same gas generant composition without inclusion of the at least one transition metal complex of diammonium bitetrazole.
  • the prior art generally fails to provide gas generant compositions, particularly non-azide gas generant compositions that are capable of simultaneously providing or resulting in relatively high gas yields, as well as sufficient and desirably high burn rates while avoiding or minimizing production or yield of undesirable inflation gas constituents such as one or more of hydrogen chloride, carbon monoxide, ammonia, nitrogen dioxide and nitric oxide.
  • gas generant compositions that are conducive or easily adaptable to manufacture or production by alternative techniques such as via extrusion processing.
  • a gas generant composition that includes: about 5 to about 60 composition weight percent of guanidine nitrate; about 10 to about 60 composition weight percent of a combination of basic copper nitrate aminotetrazole adduct, copper diammonium bitetrazole and basic copper nitrate co- oxidizer; and about 1 to about 20 composition weight percent of a polymeric binder effective to impart sufficient cohesive properties to the gas generant composition whereby the gas generant composition is extrudable.
  • a gas generant composition can desirably be extrudably processed.
  • references to a specific composition, component or material as a "fuel” are to be understood to refer to a chemical which generally lacks sufficient oxygen to burn completely to CO 2 , H 2 O and N 2 .
  • references herein to a specific composition, component or material as an "oxidizer” are to be understood to refer to a chemical generally having more than sufficient oxygen to burn completely to CO 2 , H 2 O and N 2 .
  • Burn rate enhanced material refers to materials or compositions which exhibit a bum rate of at least 0.85 inches per second at 3000 pounds per square inch (psi) or greater, preferably a burn rate of greater than about 1 inch per second at 3000 psi and, more preferably a burn rate of greater than about 1.2 inches per second at 3000 psi.
  • the term "equivalence ratio” is understood to refer to the ratio of the number of moles of oxygen in a gas generant composition or formulation to the number of moles needed to convert hydrogen to water, carbon to carbon dioxide, and any metal to the thermodynamically predicted metal oxide.
  • a gas generant composition having an equivalence ratio greater than 1.0 is over-oxidized
  • a gas generant composition having an equivalence ratio less than 1.0 is under-oxidized
  • a gas generant composition having an equivalence ratio equal to 1.0 is perfectly oxidized.
  • the gaseous effluent or inflation gas produced by the combustion of the gas generant composition is substantially free of hydrogen chloride if it includes about 5 parts per million hydrogen chloride or less when the inflator is discharged into a 100 ft 3 tank, is substantially free of carbon monoxide if it includes about 461 parts per million carbon monoxide or less when the inflator is discharged into a 100 ft 3 tank; is substantially free of ammonia if it includes about 35 parts per million ammonia or less when the inflator is discharged into a 100 ft 3 tank; is substantially free of nitrogen dioxide if it includes about 5 parts per million nitrogen dioxide or less when the inflator is discharged into a 100 ft 3 tank; and is substantially free of nitric oxide if it includes about 75 parts per million nitric oxide or less when the inflator is discharged into a 100 ft 3 tank.
  • the Figure is a simplified schematic, partially broken away, view illustrating the deployment of an airbag cushion from an airbag module assembly within a vehicle interior, in accordance with one embodiment of the invention.
  • such a gas generant composition such as for use in the inflation of inflatable elements such as an airbag cushion of an automobile inflatable restraint system.
  • a gas generant composition includes a substituted basic metal nitrate including a reaction product of an acidic organic compound and a basic metal nitrate.
  • non-azide or azide-free materials having an acidic hydrogen will react with a basic metal nitrate such as basic copper nitrate and partially replace the hydroxyl groups in the basic metal nitrate without liberating soluble metal nitrate, hi other words, the structural integrity of the basic metal nitrate is not compromised by the substitution reaction.
  • the material used desirably includes a substituted basic metal nitrate including a reaction product of an acidic organic compound and a basic metal nitrate.
  • the acidic organic compound is a nitrogen- containing heterocyclic compound including an acidic hydrogen.
  • suitable acidic organic compounds include, but are not limited to, tetrazoles, imidazoles, imidazolidinone, triazoles, urazole, uracil, barbituric acid, orotic acid, creatinine, uric acid, hydantoin, pyrazoles, derivatives thereof, and combinations thereof.
  • Particularly suitable acidic organic compounds include tetrazoles, imidazoles, derivatives thereof, and combinations thereof.
  • Examples of such acidic organic compounds include 5- amino tetrazole, bitetrazole dihydrate, and nitroimidazole.
  • the acidic organic compound includes 5-amino tetrazole.
  • basic metal nitrate compounds utilized in certain embodiments include basic metal nitrates, basic transition metal nitrate hydroxy double salts, basic transition metal nitrate layered double hydroxides, and combinations thereof.
  • Examples of basic metal nitrates include, but are not limited to, basic copper nitrate, basic zinc nitrate, basic cobalt nitrate, basic iron nitrate, basic manganese nitrate and combinations thereof, hi accordance with certain preferred embodiments, the basic metal nitrate includes basic copper nitrate.
  • a few representative substitution reactions, such as reactions (1) through (4) below, and substituted basic metal nitrate reaction products, particularly, 5-amino tetrazole substituted basic copper nitrate, bitetrazole dihydrate substituted basic copper nitrate, and nitroimidazole substituted basic copper nitrate, within the scope of the present invention are as follows:
  • the described substituted basic metal nitrate materials may be utilized as a pyrotechnic composition such as may be included in an inflator device of an automobile inflatable restraint system.
  • the described substituted basic metal nitrate materials may be used in a pyrotechnic composition such as an igniter composition or a gas generant composition including additional components such as a co-fuel, hi accordance with certain preferred embodiments, the substituted basic metal nitrate can desirably serve to enhance the burn rate of an associated gas generant composition.
  • such pyrotechnic compositions include a substituted basic metal nitrate and a nitrogen containing co-fuel.
  • burn rate enhanced gas generant compositions include a reaction product of a basic metal nitrate such as basic copper, zinc, cobalt, iron and manganese nitrates, basic transition metal nitrate hydroxy double salts, basic transition metal nitrate layered double hydroxides, and combinations thereof and an acidic organic material such as tetrazoles, tetrazole derivatives, and combinations thereof.
  • such pyrotechnic compositions may desirably include about 5 to about 60 composition weight percent co-fuel, preferably a non-azide, organic, nitrogen-containing fuel such as suited for vehicular inflatable safety restraint applications.
  • One particularly preferred pyrotechnic composition includes about 5 to about 60 composition weight percent guanidine nitrate co-fuel.
  • the desirability of use of guanidine nitrate in the pyrotechnic compositions of the invention is generally based on a combination of factors such as relating to cost, stability (e.g., thermal stability), availability and compatibility (e.g., compatibility with other standard or useful pyrotechnic composition components, for example).
  • certain preferred gas generant compositions desirably involve the addition or inclusion of a quantity of at least one transition metal complex of diammonium bitetrazole to the gas generant formulation.
  • Suitable transition metals for use in the practice of the invention include copper, zinc, cobalt, iron, nickel and chromium. Preferred transition metals include zinc and copper.
  • a copper complex of diammonium bitetrazole having an empirical formula of CuC 2 H 6 N 10 is a preferred transition metal complex of diammonium bitetrazole for use in certain preferred embodiments.
  • the invention can desirably be practice via the inclusion of a sufficient quantity of at least one transition metal complex of diammonium bitetrazole to the gas generant formulation such that the resulting formulation exhibits a desirable decrease in burn rate pressure sensitivity, as compared to the same formulation without the inclusion of such transition metal complex of diammonium bitetrazole.
  • a gas generant formulation in accordance with a preferred practice of the invention to include or incorporate the at least one transition metal complex of diammonium bitetrazole in a relative amount of at least 2 wt.%, preferably at least 5 wt.% and, more preferably, in a relative amount of at least 10 wt.% in order to provide gas generant formulations evidencing a sufficiently decreased burn rate pressure sensitivity, as may desired for at least certain such inflatable restraint system applications.
  • a pyrotechnic composition in accordance with the invention may advantageously include an additional oxidizer in an amount of up to about 50 composition weight percent.
  • additional oxidizer materials are sometimes termed "a co-oxidizer.”
  • co-oxidizers materials include basic metal nitrates, such as basic copper nitrate, metal oxides, such as cupric oxide and ferric oxide, for example, as well as ammonium perchlorate, alkali metal perchlorate, strontium nitrate, basic copper carbonate and combinations of two or more of such preferred co-oxidizer materials of basic metal nitrates, metal oxides, ammonium perchlorate, alkali metal perchlorate, strontium nitrate and basic copper carbonate.
  • such perchlorate materials for inclusion in particular subject gas generant compositions be included or present in a relative amount of about 1 to about 10 composition weight percent and have a mean particle size in excess of 100 microns and, preferably, a mean particle size of at least about 200 microns can dramatically improve the effluent resulting from the combustion of a gas generant composition which includes such sized perchlorate particles, as compared to the effluent resulting from the combustion of the same gas generant composition but without the so sized perchlorate particles.
  • it has been found advantageous that such perchlorate particles included in gas generant compositions in accordance with the invention have a mean particle size in the range of about 350 to about 450 microns.
  • Gas generant composition in accordance with the invention and suited for extrusion processing desirably also include a binder component.
  • the binder component is a polymeric binder material effective to impart sufficient cohesive properties to the gas generant composition whereby the gas generant composition is extradable.
  • Extrudable gas generant compositions in accordance with certain preferred embodiments will desirably include or contain about 1 to about 20 composition weight percent of such a polymeric binder component.
  • suitable binder materials can include cellulosics, natural gums, polyacrylates, polyacrylamides, polyurethanes, polybutadienes, polystyrenes, polyvinyl alcohols, polyvinyl acetates, silicones and combinations of two or more thereof. More particularly, suitable cellulosic binder materials may include ethyl cellulose, carboxymethyl cellulose, hydroxylpropyl cellulose and combinations of two or more thereof. Suitable natural gum binder materials may include guar, xanthan, arabic and combinations of two or more thereof.
  • binder materials such as the above-described cellulosic binders, that result in or form compositions that burn at lower temperatures, sometimes referred to as "cooler burning” materials, can be advantageously preferred for various applications.
  • gas generant compositions prepared via extrusion processing can desirably exhibit increased or maximized loading densities such as may desirably serve to reduce or minimize the required chamber volume associated therewith.
  • extruded gas generant compositions may further desirably more easily burn at higher pressure conditions and can thus serve to reduce or minimize the production or yield of incomplete products of combustion such as having the general form of CO x and NO x , for example.
  • One or more of the materials or ingredients included in the subject compositions may serve multiple roles or functions in particular formulations.
  • binder materials can also typically act or function as a fuel components, as above defined.
  • specific range limits for particular materials includable in the subj ect compositions are generally dependent, at least in part, on what other particular materials are included in a specific composition.
  • Such specific range limits for particular materials includable in the subject compositions are readily identifiable by those skilled in the art and guided by the teachings herein provided Additional additives such as slag forming agents, flow aids, plasticizers, viscosity modifiers, pressing aids, dispersing aids, or phlegmatizing agents may also be included in the pyrotechnic composition to facilitate processing or to provide enhanced properties!
  • pyrotechnic compositions in accordance with the invention may include a slag forming agent such as a metal oxide compound such as aluminum oxide.
  • a slag forming agent such as a metal oxide compound such as aluminum oxide.
  • such additives may be included in the subject compositions in an amount of about 1 to no more than about 5 composition weight percent.
  • Such additives typically are one or more metal oxide materials, with preferred such additives including metal oxides such as silicon dioxide, aluminum oxide, zinc oxide, and combinations thereof.
  • gas generating compositions such as herein above-described desirably provide or result in a burn rate of greater than about 0.85 inches per second at 3000 psi, preferably a burn rate of greater than about 1 inch per second at 3000 psi and, more preferably a burn rate of greater than about 1.2 inches per second at 3000 psi.
  • gas generating compositions such as herein above-described desirably provide or result in a burn rate pressure sensitivity (as represented by the pressure exponent (n) in the burn rate equation (1) identified above) of less 0.5, preferably of less than about 0.48. Still further, gas generating compositions such as herein above-described desirably provide or exhibit a combustion flame temeprature of less than 2000 K.
  • gas generating compositions in accordance with the invention can be incorporated, utilized or practiced in conjunction with a variety of different structures, assemblies and systems.
  • the Figure illustrates a vehicle 10 having an interior 12 wherein an inflatable vehicle occupant safety restraint system, generally designated by the reference numeral 14, is positioned.
  • an inflatable vehicle occupant safety restraint system generally designated by the reference numeral 14
  • certain standard elements not necessary for an understanding of the invention may have been omitted or removed from the Figure for purposes of facilitating illustration and comprehension.
  • the vehicle occupant safety restraint system 14 includes an open-mouthed reaction canister 16 which forms ahousing for an inflatable vehicle occupant restraint 20, e.g., an inflatable airbag cushion, and an apparatus, generally designated by the reference numeral 22, for generating or supplying inflation gas for the inflation of an associated occupant restraint.
  • a gas generating device is commonly referred to as an "inflator.”
  • the inflator 22 contains a quantity of a gas generant composition in accordance with the invention and such as described above.
  • the inflator 22 also includes an ignitor, such as known in the art, for initiating combustion of the gas generating composition in ignition communication with the gas generant composition.
  • the airbag cushion 20 upon deployment desirably provides for the protection of a vehicle occupant 24 by restraining movement of the occupant in a direction toward the front of the vehicle, i.e., in the direction toward the right as viewed in the Figure.
  • the present invention is described in further detail in connection with the following examples which illustrate or simulate various aspects involved in the practice of the invention. It is to be understood that all changes that come within the spirit of the invention are desired to be protected and thus the invention is not to be construed as limited by these examples.
  • Example land Comparative Examples 1-3 500 pound batches of each of the gas generant formulations having the compositions (values are in weight percent) identified in TABLE 1 below were prepared in the following manner:
  • Comparative Example 1 Guanidine nitrate (GN) was dissolved in approximately 30% water (i.e., 30% as a percentage of the total solids in mix on a wet basis, i.e., 214 lbs water) at 190 °F.
  • Basic carbon nitrate (bCN), alumina and silica were added thereto to make a slurry.
  • the slurry was pumped through a lance and sprayed into a drying tower where it dried to a powder as it fell from the top to the bottom of the drying tower.
  • Example 1 The same procedure as in Comparative Example 1 was followed except that cupric oxide and diammonium bitetrazole were reacted in water at 190° F for 1 hour in order to make the copper diammonium bitetrazole prior to the addition of the other ingredients.
  • cupric oxide and diammonium bitetrazole were reacted in water at 190° F for 1 hour in order to make the copper diammonium bitetrazole prior to the addition of the other ingredients.
  • GN guanidine nitrate
  • bCN basic copper nitrate
  • the gas generant formulation of each of Comparative Examples 1-3 and Example 1 was then tested.
  • the burn rate and combustion flame temperature (T 0 ) values identified in TABLE 2 below were obtained.
  • the burn rate data was obtained by first pressing samples of the respective gas generant formulations into the shape or form of a 0.5 inch diameter cylinder using a hydraulic press (12,000 lbs force). Typically enough powder was used to result in a cylinder length of 0.5 inch.
  • the cylinders were then each coated on all surfaces except the top one with a krylon ignition inhibitor to help ensure a linear burn in the test fixture, in each case, the so coated cylinder was placed in a 1 -liter closed vessel capable of being pressurized to several thousand psi with nitrogen and equipped with a pressure transducer for accurate measurement of vessel pressure.
  • a small sample of igniter powder was placed on top of the cylinder and a nichrome wire was passed through the igniter powder and connected to electrodes mounted in the vessel lid.
  • the closed vessel was then pressurized to the desired pressure and the sample ignited by passing a current through the nichrome wire. Pressure vs. time data was collected as each of the respective samples were burned.
  • the inclusion of CuDABT in CE 2 while resulting in a formulation with an increased burn rate also significantly increased the pressure sensitivity of the burning rate (as represented by the pressure exponent (n)).
  • Example 1 shows that gas generant inclusion of both bCuATN and copper diammonium bitetrazole, albeit in the relatively low relative level of 4%, provided a desirably increased or elevated burn rate while also exhibiting a desirably reduced or decreased burn rate pressure sensitivity.
  • TABLE 2 also shows that the gas generant material of Example 1 exhibited a combustion flame temperature of below 2000 K. As discussed above, with gas generant materials having a combustion flame temperature of below 2000 K undesirable effluent reactions resulting in increased levels of undesirable species such as carbon monoxide and nitrogen oxides can be avoided or minimized.
  • non-azide or azide-free gas generant materials or compositions are provided that, while overcoming at least some of the potential problems or shortcomings of azide-based pyrotechnic compositions, may also provide relatively high gas yields as compared to typical azide-based pyrotechnic compositions.
  • These gas generant compositions also desirably provide or result in a sufficient and desirably high burn rate, e.g., a burn rate of greater than about 0.85 inches per second at 3000 psi, preferably a burn rate of greater than about 1 inch per second at 3000 psi and, more preferably a burn rate of greater than about 1.2 inches per second at 3000 psi.
  • gas generant compositions are particularly adapted and well-suited for extrudable production and can thus provide new or facilitate alternative economic and efficient gas generant production techniques. Furthermore, such gas generant compositions can attain or permit desirably increased or maximized loading densities such as to reduce or minimize the required chamber volume associated therewith.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Air Bags (AREA)

Abstract

La présente invention concerne une composition générant des gaz qui inclut un combustible organique contenant de l'azote autre qu'un azide, un nitrate basique de métal substitué et au moins un complexe à métal de transition de diammonium bitétrazole. Le nitrate basique de métal substitué peut être le produit d'une réaction entre un composé organique acide et un nitrate basique de métal. Le complexe à métal de transition de diammonium bitétrazole est capable d'améliorer efficacement la sensibilité à la pression du taux de combustion de la composition générant des gaz par comparaison avec la même composition générant des gaz sans inclusion d'au moins un complexe à métal de transition du diammonium bitétrazole.
PCT/US2006/032422 2005-09-13 2006-08-18 Matières générant des gaz WO2007032862A2 (fr)

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US11/225,692 US20060054257A1 (en) 2003-04-11 2005-09-13 Gas generant materials
US11/225,692 2005-09-13

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