USRE45899E1 - Low temperature, extrudable, high density reactive materials - Google Patents
Low temperature, extrudable, high density reactive materials Download PDFInfo
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- USRE45899E1 USRE45899E1 US12/507,605 US50760509A USRE45899E US RE45899 E1 USRE45899 E1 US RE45899E1 US 50760509 A US50760509 A US 50760509A US RE45899 E USRE45899 E US RE45899E
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- reactive material
- tetrafluoroethylene
- metal
- fluoropolymer
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F42—AMMUNITION; BLASTING
- F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
- F42B1/00—Explosive charges characterised by form or shape but not dependent on shape of container
- F42B1/02—Shaped or hollow charges
- F42B1/032—Shaped or hollow charges characterised by the material of the liner
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B27/00—Compositions containing a metal, boron, silicon, selenium or tellurium or mixtures, intercompounds or hydrides thereof, and hydrocarbons or halogenated hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F42—AMMUNITION; BLASTING
- F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
- F42B12/00—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material
- F42B12/02—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect
- F42B12/20—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect of high-explosive type
- F42B12/22—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect of high-explosive type with fragmentation-hull construction
- F42B12/32—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect of high-explosive type with fragmentation-hull construction the hull or case comprising a plurality of discrete bodies, e.g. steel balls, embedded therein or disposed around the explosive charge
Definitions
- This invention relates generally to a reactive material suitable for use as a shape-charge liner in a penetrating warhead and in reactive fragments in a fragmentary warhead. More specifically, the invention relates to a reactive material comprising a fluoropolymer and a metal filler. This reactive material is capable of being safely processed at temperatures significantly below the thermal autoignition point of the reactive material.
- a penetrating warhead 2 used in a projectile or missile typically comprises a case 4 , an explosive material 6 , an initiator, and a liner 8 , as shown in FIG. 1A .
- the case 4 is generally a cylindrical tube comprised of steel, plastic, or a composite material. At least a portion of the case 4 is typically filled with the explosive material 6 .
- the liner 8 forms a high-velocity jet that has a high kinetic energy capable of penetrating solid objects, such as a target.
- the liner 8 is formed from a solid material that is formed into a jet responsive to detonation of the explosive charge.
- the liner material is typically a high density, ductile material, such as a metal, a metal alloy, a ceramic, or a glass.
- the metals commonly used in liners include copper, aluminum, depleted uranium, tungsten, or tantalum.
- fragmentary warheads 10 are commonly used. As illustrated in FIG. 1B , the fragmentary warhead 10 typically comprises fragments 12 of material that are projected at a target upon detonation of the explosive material 6 of the warhead 10 .
- the fragments 12 must be able to withstand the explosive force of the detonation, otherwise the force commonly breaks up the fragments, thereby reducing their ability to penetrate the target.
- the liner 8 or fragments 12 may be provided with the ability to produce secondary reactions that cause additional damage. These secondary reactions commonly include incendiary reactions.
- pyrophoric metals are added to the liner to provide the desired incendiary effects.
- a double-layered liner is disclosed, where a layer of dense metal provides the penetration ability and a layer of light metal, such as aluminum or magnesium, produces the incendiary effects.
- reactive material refers to a material comprising a metal that reacts with an oxidizing agent. Upon impact with a target, the reactive material of the liner produces a high burst of energy.
- a known reactive material includes an aluminum and polytetrafluoroethylene (“PTFE”) material, referred to herein as an “Al/PTFE” reactive material.
- PTFE is available from DuPont under the tradename TEFLON®. PTFE has the highest fluorine content of all fluoropolymers, is the most resistant fluoropolymer to chemical attack, and requires high processing temperatures to achieve its maximum strength.
- PTFE is used in reactive materials because its high fluorine content makes it a strong oxidizing agent.
- the Al/PTFE reactive material has good penetration ability in light armor or thin-skinned targets, such as aircraft, due to the density of the aluminum.
- the Al/PTFE reactive material also provides incendiary reactions because the reactive material ignites upon penetration into the target.
- the reactive material is pressed into billets or pressed preforms.
- the pressed preforms are then sintered and annealed at high temperatures, typically 350-390° C. Due to PTFE's high melting temperature of 342° C., these high sintering temperatures are necessary to form reactive materials using PTFE.
- the currently preferred technique for forming Al/PTFE fragments comprises blending the PTFE and aluminum in a solvent.
- the solution of Al/PTFE is spread on a tray and dried in an oven. The dried composition is then conditioned to 185° F. and pressed in a 185° F. heated die. The pressed preform is then heated to 350-390° C.
- the sintered preform is then cooled at a set rate to minimize cracking and maximize the mechanical properties of the Al/PTFE reactive material.
- the mechanical properties of the Al/PTFE reactive material are inversely related to the degree of crystallinity in the PTFE. In general, high crystallinity in the PTFE results in low tensile strength and high elongation.
- the current processing techniques available to form high strength components from Al/PTFE are limited due to PTFE's high viscosity at the 350-390° C. temperatures required for sintering.
- reactive materials comprising PTFE and metals with a higher density than aluminum have been produced.
- These higher density metals included tantalum and tungsten, which are more chemically reactive with PTFE at the sinter temperatures than aluminum.
- These Ta/PTFE and W/PTFE reactive materials were processed, using the same conditions as the Al/PTFE reactive material, to form 3.5-inch diameter and 1-inch diameter pucks.
- the Ta/PTFE and W/PTFE reactive materials exhibited undesirable grain cracking resulting from volatile chemical reactions during the sintering process.
- the tungsten and tantalum reacted with trace amounts of hydrofluoric acid (“HF”) present at the temperatures used during the sintering process to produce highly volatile reaction products.
- HF hydrofluoric acid
- the Ta/PTFE reactive material formed volatile tantalum fluoride compounds that were extremely exothermic. Accelerated Rate calorimetry (“ARC”) testing of the Ta/PTFE material revealed an exotherm that occurred at only a few degrees higher than the sintering temperature. This exotherm occurred at 375° C. In addition, the strong exothermic reaction caused the Ta/PTFE reactive material to autoignite at 307° C. during an experimental sinter cycle. The W/PTFE reactive material off-gassed during the sintering process due to the formation of highly volatile tungsten fluoride compounds (such as WF 6 and WOF 4 ) that caused severe cracking of the pressed preforms. These highly exothermic reactions raised concerns regarding the safety of processing the Ta/PTFE reactive materials at the high temperatures necessary to process PTFE. The highly exothermic reactions also raised concerns regarding the quality of the W/PTFE reactive materials due to the observed cracking.
- ARC Accelerated Rate calorimetry
- Reactive materials comprising a metal and a fluoropolymer have also been used in military pyrotechnics.
- U.S. Pat. No. 5,886,293 to Nauflett et al. a process of producing energetic materials for use in military pyrotechnics is disclosed.
- the energetic material comprises a magnesium fluoropolymer, specifically magnesium/TEFLON®/Viton® (“MTV”).
- MTV magnesium/TEFLON®/Viton®
- Viton® is a copolymer of vinylidenefluoride-hexafluoropropylene.
- the resulting energetic material is used to produce rocket motor igniters and aircraft decoy flares.
- the present invention relates to a reactive material comprising at least one metal filler and an oxidizing agent.
- the oxidizing agent comprises a fluoropolymer having a high fluorine content, a low melt temperature, and a high mechanical strength.
- the fluoropolymer is a thermoplastic fluoropolymer, such as a polymer of tetrafluoroethylene, hexafluoropropylene, and vinylidene fluoride.
- the metal filler comprises a high density, reactive metal, such as hafnium, tantalum, magnesium, titanium, tungsten, aluminum, magnesium/aluminum alloys, or zirconium.
- the metal filler may be a metal/metal oxide filler or an intermetallic filler.
- the reactive material is processed at temperatures significantly below the thermal autoignition point of the reactive material.
- the present invention also relates to an article, such as a warhead, comprising the reactive material.
- the present invention relates to a method of safely processing a reactive material.
- the method comprises mixing at least one metal filler with an oxidizing agent to form the reactive material.
- the reactive material is then processed at a temperature below the thermal autoignition point of the reactive material.
- FIGS. 1A and 1B schematically illustrate a penetrating warhead and a fragmentary head
- FIG. 2 shows ARC temperature and pressure v. time plots for a step heat run performed on a composition of Ta/THV 220;
- FIG. 3 shows ARC temperature and pressure v. time plots for a 250° C./24 hour isothermal age run performed on a composition of Ta/THV 220;
- FIGS. 4 and 5 show ARC temperature and pressure v. time plots for a 200° C./24 hour isothermal age run performed on different sample sizes of a composition of Ta/THV 220;
- FIG. 6 shows ARC temperature and pressure v. time plots for a step heat run performed on a composition of Hf/THV 220;
- FIG. 7 shows ARC self-heat rate v. temperature plots for a step heat run performed on a composition of Hf/THV 220.
- FIG. 8 shows thermal stability results for a 200° C./24 hour isothermal age run performed on a composition of Hf/THV 220.
- the reactive material of the present invention may be used as a reactive liner 8 in penetrating (shape-charge) warheads 2 and in high strength reactive fragments 12 in fragmentary warheads 10 , as illustrated in FIGS. 1A and 1B .
- the reactive material comprises an oxidizing and at least one metal filler and may be safely processed at temperatures significantly below the thermal autoignition point of the reactive material.
- the reactive fragments 12 and reactive liners 8 are able to penetrate solid targets and produce incendiary effects after the fragments/liners have penetrated the target, thereby increasing the destructive effect of the warheads.
- the oxidizing agent may provide strength to the reactive material so that the reactive material survives detonation of the warhead.
- the oxidizing agent may be a strong oxidizer so that secondary reactions, such as incendiary reactions, occur when the reactive material penetrates its target.
- the incendiary reactions may also be due to afterburning of the metal filler, which is caused by a reaction between the metal filler and atmospheric oxygen.
- the oxidizing agent may accelerate the rate of metal filler/atmospheric oxygen reaction.
- the oxidizing agent is a fluoropolymer or fluoroelastomer with a high fluorine content, a low melt temperature, and a high mechanical strength. More preferably, the oxidizing agent is a thermoplastic fluoropolymer.
- the high mechanical strength of the fluoropolymer may provide the reactive material with the strength to survive the detonation or explosive launch of the warhead.
- the mechanical strength of the fluoropolymer may be particularly important in fragmentary warheads 10 because coherent fragments 12 must survive the detonation in order to impact the target.
- the high fluorine content of the fluoropolymer may provide the necessary oxidizing strength to produce incendiary reactions with the metal filler when the reactive material penetrates its target.
- the heat generated when the reactive material penetrates the target may cause the fluorines in the fluoropolymer to be liberated from the hydrocarbon chain of the fluoropolymer and to exothermically react with the metal filler.
- the low melt temperature of the fluoropolymer may help to ensure that the reactive material may be processed at a temperature below which the rate of metal reacting with trace amounts of HF is greatly reduced or eliminated.
- the melting temperature of the fluoropolymer may not exceed the autoignition temperature of the reactive material (the fluoropolymer/metal filler composition). In other words, the reactive material may not produce an exotherm or exotherms at or below the processing temperature.
- the processing temperature of the reactive metal may vary depending on the melting point of the fluoropolymer and the amount of metal filler present. To provide an adequate margin of safety, the processing temperature may be no higher than 50° C. below the thermal autoignition point of the reactive material or the temperature at which an exotherm occurs. However, depending on the acceptable degree of risk in processing the reactive materials, this 50° C. margin of error may be reduced as long as the melting temperature of the fluoropolymer does not exceed the autoignition temperature of the reactive material.
- the fluoropolymer of the reactive material may be selected based on its low-temperature processing capability, cost, availability, fluorine content, mechanical properties of the unfilled fluoropolymer, melting point, viscosity at desired processing temperature, and compatibility of the fluoropolymer with reactive metal fillers. Properties of selected commercially available fluoropolymers are shown in Table 1. These fluoropolymers are available from Dupont, Dyneon LLC, and Asahi Glass Co., Ltd.
- the fluoropolymer of the present invention may include, but is not limited to, a thermoplastic terpolymer of tetrafluoroethylene, hexafluoropropylene, and vinylidene fluoride (“THV”), a thermoplastic copolymer of tetrafluoroethylene and perfluorovinylether (“PFA”), a thermoplastic copolymer of tetrafluoroethylene and ethylene (“ETFE”), or a thermoplastic copolymer of tetrafluoroethylene and hexafluoropropylene (“FEP”).
- TSV thermoplastic terpolymer of tetrafluoroethylene, hexafluoropropylene, and vinylidene fluoride
- PFA thermoplastic copolymer of tetrafluoroethylene and perfluorovinylether
- ETFE thermoplastic copolymer of tetrafluoroethylene and ethylene
- FEP thermoplastic copolymer of
- one fluoropolymer as the oxidizing agent, it is also contemplated that a combination of at least two fluoropolymers may be used.
- a combination of PTFE and THV 220 or a combination of two different THV polymers may be used.
- At least two fluoropolymers may be present in percentages sufficient to provide the high fluorine content, the low melt temperature, and the high mechanical strength to the reactive material.
- the fluorine content of the fluoropolymer is preferably greater than approximately 45% by weight.
- a fluoropolymer having a lower fluorine may be used depending on the mechanical properties of the fluoropolymer.
- a fluoropolymer having a fluorine content less than approximately 45% by weight may be used if the fluoropolymer has a high tensile strength and a high percentage of elongation, in addition to the desired low melt temperature.
- the fluoropolymer of the reactive material is THV 220, available from Dyneon LLC (Oakdale, Minn.), because THV 220 is easy to process due to its complete solubility in conventional solvents and its low melt temperature.
- THV 220 has a melt temperature of 222° C. below the melt temperature of PTFE.
- Conventional solvents include ketones and esters and, more specifically, acetone and ethyl acetate.
- the low melt temperature of THV 220 allows the reactive material to be processed at temperatures significantly below the thermal autoignition point using conventional batch mixers.
- THV 220 is further preferable because the sintering process required to produce PTFE reactive materials may be eliminated, thereby increasing production efficiency.
- THV polymers including, but not limited to, THV X 310, THV 415, THV 500, and HTEX 1510, all available from Dyneon LLC, may be used as the fluoropolymer of the reactive material.
- THV polymers including, but not limited to, THV X 310, THV 415, THV 500, and HTEX 1510, all available from Dyneon LLC.
- THV polymers may be used as the fluoropolymer of the reactive material.
- the primary advantage offered by THV polymers is the significantly reduced process temperature and the elimination of the sintering process required in PTFE processing.
- Other fluoropolymers may also be used in the reactive material as long as these fluoropolymers have the desired properties of a high fluorine content, a low melt temperature, and a high mechanical strength.
- the metal filler of the reactive material may be a reactive, high density metal that provides the requisite penetrating power and energy release for the warhead.
- the metal filler may be magnesium, aluminum, magnesium/aluminum alloys, iron, copper, zirconium, titanium, zinc, boron, silicon, manganese, tin, hafnium, tungsten, depleted uranium, or tantalum, or metal carbides, oxides, or nitrides of these metals.
- the metal filler may have a density that is approximately equal or greater than the density of magnesium (1.74 g/cm 3 ).
- the metal filler may be at least as reactive with the oxidizing agent as magnesium or aluminum.
- the metal filler is hafnium, tantalum, magnesium, titanium, tungsten, aluminum, magnesium/aluminum alloys, or zirconium.
- the metal fillers may be combined with the reactive material in powdered form.
- intermetallic thermitic and incendiary mixes of the metal filler may also be used within the scope of the invention.
- the metal filler may also be a combination or blend of two or more of these metals.
- the metal filler may be a blend of hafnium and tantalum.
- the metal filler may be a metal/metal oxide filler (a thermite), such as Fe 2 O 3 /aluminum, Fe 2 O 3 /zirconium, CuO/aluminum, Fe 2 O 3 /titanium, tantalum/iron oxide, manganese dioxide/aluminum, or other thermite compositions.
- a thermite such as Fe 2 O 3 /aluminum, Fe 2 O 3 /zirconium, CuO/aluminum, Fe 2 O 3 /titanium, tantalum/iron oxide, manganese dioxide/aluminum, or other thermite compositions.
- Intermetallic fillers that include a blend of two or more of the metals may also be used.
- the intermetallic fillers may include a blend of unreacted metals that have differing numbers of molar ratios of each of the two or more metals, such as one mole of hafnium and two moles of aluminum; one mole of hafnium and one mole of aluminum; one mole of hafnium and two moles of boron; one mole of nickel and one mole of aluminum; one mole of titanium and one mole of aluminum; one mole of titanium and two moles of aluminum; one mole of titanium and two moles of aluminum; one mole of zirconium and one mole of aluminum; one mole of zirconium and two moles of aluminum; one mole of molybdenum and two moles of aluminum; one mole of aluminum and two moles of boron; one mole of hafnium and two moles of boron; one mole of tantalum and one mole of boron; one mole of titanium and two moles of boron; one mole of zirconium and one mole
- the fluoropolymer may be present in the reactive material at approximately 15-90% by weight. Preferably, the fluoropolymer is present at approximately 25-75% by weight.
- the metal filler may be present at approximately 10-85% by weight.
- the reactive material may be produced by mixing the fluoropolymer and the metal filler, as known in the art. If the fluoropolymer is soluble in ketones or esters, a particle size of the fluoropolymer may not be critical to the operability of the present invention. However, if the fluoropolymer is insoluble in ketones or esters, the fluoropolymer may be commercially obtained in milled form or may be processed to its milled form, as known in the art. The insoluble fluoropolyner preferably has a small particle size, such as an average particle size of approximately 1 micron. The fluoropolymer may then be combined with the metal filler and blended with a solvent to form a suspension of reactive material.
- a twin-screw extruder may also be used to compound or mix the metal filler with the fluoropolymer if solvents are undesirable. If the fluoropolymer is soluble in ketones or esters, the reactive material may be mixed by a solvent loss technique or a polymer precipitation technique, which are described in more detail below.
- the reactive material may be processed by pressing or extrusion to manufacture near-net-shape preforms.
- a reactive material comprising a fluoropolymer that is insoluble in ketones or esters may be directly pressed or extruded, as described below.
- a reactive material comprising a soluble fluoropolymer may be processed by the polymer precipitation or solvent loss techniques, followed by pressing or extrusion. If the reactive material is processed by pressing, the solution of reactive material is dried in an oven. The dried reactive material is then loaded into a die that is heated to approximately 165-180° C. This temperature is dependent on the melting point and the viscosity of the reactive material.
- the reactive material is melted under pressure (approximately 1500 psi) and under vacuum. This pressure is dependent on the rheology of the reactive material.
- the die is cooled to below the melt temperature of the die (approximately 80-100° C.) for several minutes.
- the pressing pressure is then increased to approximately 3000-4000 psi and the cooling of the die is continued to 50-60° C. It is essential that the die have a slow cooling rate to maximize polymer crystallinity and mechanical properties.
- the solution of reactive material is dried in an oven.
- the dried reactive material is then loaded into an extruder heated to approximately 165-180° C.
- the reactive material is melted under pressure (approximately 1500 psi) and under vacuum.
- the pressure required to melt the reactive material is dependent on the fluoropolymer used in the reactive material and the metal content in the reactive material.
- the extrusion pressure is then increased to form an extrudate, which is then cut into pieces and allowed to cool to ambient room temperature.
- these reactive materials may be used to allow near-net-shape fabrication of components using injection molding or extrusion, thereby reducing waste and machining time.
- the processed reactive materials formed by either of these methods may be analyzed to determine the percentage of theoretical maximum density (“% of TMD”) for each reactive material.
- the % of TMD is measured as known in the art. If the reactive material has a % of TMD equal to approximately 100%, it indicates that no voids are present in the reactive material.
- the desired % of TMD of the reactive material may range between approximately 80-100%. Preferably, the % of TMID of the reactive material is between approximately 90-100% and, more preferably, between approximately 95-100%. The desired % of TMD may depend on the ultimate application in which the reactive material may be used.
- the reactive material having a sufficient % of TMD may be used in reactive fragments 12 for fragmentary warheads 10 or liners 8 in penetrating warheads 2 .
- the reactive material may be machined, pressed, or extruded into a desired shape for use as the liner 8 .
- the reactive material may be placed into a mold to produce the desired shape of the liner 8 .
- the reactive material is weighed into the desired quantity.
- TEFLON® tape is placed on a top surface of a first copper dish and a bottom surface of a second copper dish. The first copper dish is heated in a 170° C. oven.
- a TEFLON® brick is placed over the first copper dish and the reactive material is stacked into the middle of the first copper dish.
- the reactive material is heated for about 45 minutes or until it becomes easily pliable.
- the second copper dish is placed on top of the material and lightly pressed down, making sure that the alignment of the dish is flat.
- a TEFLON® donut is placed on top of the second copper dish and two metal weights are placed on top of the TEFLON® donut.
- the TEFLON® donut and metal weights are arranged so that the weight is pressing straight down on the reactive material to ensure that the reactive material will have a uniform thickness.
- the set-up is left for 45 minutes in the oven and then removed.
- the mold is removed from the TEFLON® brick and cooled for 15 minutes.
- the two copper dishes are then pried off, thereby releasing a liner formed from the reactive material in the desired shape.
- the liner may be formed into a shape up to several inches thick.
- a fragmentary warhead 10 which comprises fragments 12 of reactive material
- the reactive material may be processed into the desired fragment shapes by extrusion or pressing.
- These reactive fragments 12 may have a thickness up to several inches thick.
- the dimensions of a liner 8 or reactive fragments 12 may vary, depending on the application in which the reactive material is being used. Therefore, each application may require optimization testing.
- the reactive material of the present invention may be deposited in the warhead as known in the art.
- the reactive material may replace the conventional liner 8 , such as the copper liner, that is used in penetrating warheads 2 .
- the reactive material may be used in addition to the copper liner.
- the reactive material may be deposited on top of the copper liner.
- the reactive material may also be formed into reactive fragments 12 for use in a fragmentary warhead 10 . These reactive fragments 12 may be secured in the warhead as known in the art.
- the reactive materials of the present invention significantly reduce or eliminate the safety concerns associated with the processing of high density, reactive metals and fluoropolymers. These reactive materials can be processed at dramatically lower temperatures and pressures in comparison to the temperatures and pressures required to process PTFE reactive materials. These reactive materials can also be processed more efficiently because the sintering step necessary to process PTFE is eliminated. The reactive materials also allow near-net-shape fabrication of reactive material components using injection molding or extrusion, thus reducing waste. In addition, waste is eliminated because the reactive material can be readily recycled into new components. Finally, processing of these reactive materials eliminates the use of solvent in the process as they may be mixed or compounded in a twin screw extruder.
- compositions of Ta/THV 220 and Hf/THV 220 reactive materials are shown in Table 2.
- the Ta/THV 220 reactive materials were mixed using two techniques, the solvent loss technique and the polymer precipitation technique, to determine which technique provided the best mixing. Two small 10-gram mixes were made using both techniques. In the solvent loss method, the THV 220 was dissolved in acetone. The tantalum was mixed in with the THV 220 while stirring continuously to drive off the acetone. Small chunks of homogeneous, tantalum-filled THV 220 material were produced, which were then dried in a forced-air oven. The solvent loss technique resulted in a well mixed composition of tantalum-filled THV 220. However, one disadvantage of this technique is that solvent is required when the reactive material is produced in batch mixes.
- THV 220 was dissolved in acetone and tantalum was mixed into the solution.
- a non-polar solvent such as hexane or heptane, was then added to change the polarity of the solution, forcing the THV 220 to precipitate.
- One advantage of this technique is its increased speed, which reduces the time needed for mixing.
- this process works extremely well with reactive materials that have less than 20 percent by volume of the fluoropolymer.
- the high-density Ta/THV 220 and Hf/THV 220 reactive materials contained approximately 70% by volume of THV 220, which resulted in large sticky agglomerates that were hard to process.
- the solvent loss technique was used to produce subsequent Ta/THV 220 and Hf/THV 220 reactive materials.
- a total of 3 ⁇ 1000 -gram mixes were made with tantalum and hafnium, respectively.
- Reactive materials comprising one of THV 220, THV X 310, THV 415, THV 500, or HTEX 1510 as the fluoropolymer and one of tantalum, hafnium, aluminum, magnesium, tungsten, titanium, or zirconium as the metal filler are produced as described in Examples 1 and 2.
- the weight percentage of fluoropolymer and metal filler is determined as known in the art.
- the “isofixed” algorithm was used for isothermal aging on the original ARC.
- the disadvantage to the “isotracked” mode was that the calorimeter was more likely to drift and even registered false exotherms during a long isothermal age run. Long-term temperature stability was better with the classic “isofixed” aging mode. Since some positive temperature drift problems were experienced in the “isotracked” mode, all remaining experiments were conducted in the “isofixed” mode.
- the 250° C./24 hour isothermal age run was performed on the Ta/THV 220 reactive material (using a different sample than the original run, possibly with different thermal stability characteristics) on a 5.1143 gram sample. This sample size was large enough to provide a good simulation of a bulk sample. Also, isothermal aging did a better job than step heating of unmasking initially slow autocatalytic reactions that can lead to a sudden thermal runaway.
- FIG. 3 shows the temperature versus time behavior of this sample, which autoignited after less than seven hours at 250° C. This temperature is also significantly above the temperatures that will be used to process the Ta/THV 220 reactive materials.
- FIGS. 6 and 7 show the temperature/pressure v. time and self-heat rate v. temperature curves respectively for a small (0.3109 gram) sample of Hf/THV 220 reactive material.
- a small sample of Hf/THV 220 reactive material Starting at about 275° C., there were several small exotherms with self-heat rates near the exotherm threshold (0.020° C./min) that were not sustained.
- step heating resumed, which happened several times between 275 and 355° C.
- 355° C. a sustained exotherm was finally observed.
- 355° C. is significantly above the temperatures that will be used to process the Hf/THV 220 reactive materials.
- the lower temperature exothermic behavior may have had a contribution from calorimeter drift. It is also unclear what happened to the pressure trace on this run at high temperatures.
- Reactive materials produced according to Example 3 are evaluated for thermal stability according to Example 4. Thermal stability tests are performed as described in Example 4.
- Reactive materials are obtained that have no thermal hazard potential for the proposed extrusion involving short-term exposure of these reactive materials to temperatures slightly greater than the melt temperature of the specific fluoropolymers used in the composition.
- the mixed Ta/THV 220 and Hf/THV 220 reactive materials were processed by pressing or ram extrusion. The two methods were evaluated to determine whether the method of processing affected the reactive material. Initially, the reactive material was pressed into right circular cylinders and evaluated and eliminated for safety reasons due to the large amount of flashing produced when small samples of inert THV 220 (NaCl/THV 220 and KCl/THV 220) compositions were pressed. Pressing the Al/THV 220, Ta/THV 220 and Hf/THV 200 reactive materials while they were being melted potentially presented a safety hazard due to the flashing formed around the pressing ram.
- the processed Ta/THV 220 and Hf/THV 220 extrudates were evaluated to determine the % of TMD for each sample.
- Reactive materials comprising the metal fillers and fluoropolymers described in Example 3 are processed as described in Example 6.
- the extrudates from these processed reactive materials are evaluated to determine the % of TMD for each sample.
- these Ta/THV 220 extrudates had TMD values ranging from 98.81-99.32%, with an average TMD value of 99.106%. These TMD values are significantly higher than the average TMD value for W/PTFE, which was determined to be approximately 96% (data not shown). These TMD values are also higher than the TMD values for Al/THV 220, which were determined to range from approximately 97.9%-99.2% (data not shown).
- the % of TMD values for the Hf/THV 220 extrudates were calculated and are presented in Table 5.
- the lower % of TMD may be related to changes in the reactive material's rheology or poor bonding of the THV 220 to the surface of the hafnium powder.
- the Hf/THV 220 extrudates comprised small shiny specks that were believed to be uncoated Hf particles.
- the lower density values of the Hf/THV 220 extrudate support this observation because the uncoated Hf would result in microscopic voids in the material, thereby reducing the % of TMD.
- the TMD values for the Hf/THV 220 reactive materials are slightly lower than the TMD values for the Ta/THV 220 reactive materials. However, the % of TMD for the Hf/THV 220 reactive materials are higher than the average TMD value for W/PTFE, which was determined to be approximately 96% (data not shown). These TMD values are also comparable to the TMD values for Al/THV 220, which were determined to range from approximately 97.9%-99.2% (data not shown).
- the % of TMD values for the reactive materials comprising the metal fillers and fluoropolymers described in Example 3 are measured. Reactive materials that have TMD values greater than the average TMD value for W/PTFE are obtained. The average TMD value for W/PTFE was determined to be approximately 96% (data not shown).
- the Ta/THV 220 and Hf/THV 220 reactive materials exhibited improved penetration into solid targets compared to the Ta/PTFE and W/PTFE reactive materials (data not shown).
- Reactive materials comprising the metal fillers and fluoropolymers described in Example 3 are obtained. These reactive materials have improved penetration into solid targets compared to the Ta/PTFE and W/PTFE reactive materials.
Abstract
Description
TABLE 1 |
Properties of Selected Fluoropolymers |
Tensile | (%) | Fluorine | |||
Strength | Elonga- | Melting | Content | ||
(psi) | tion at | Point | (% by | ||
Polymer | at 23° C. | 23° C. | (° C.) | Solubility | weight) |
Polytetrafluorethylene |
PTFE | 4500 | 400 | 342 | Insoluble | 76 |
(TEFLON ®) | |||||
TFM 1700 | 5800 | 650 | 342 | Insoluble | 76 |
Modified PTFE |
Fluoroelastastomers (Gums) |
Viton A | 2000 | 350 | 260 | Soluble in | 65.9 |
(Fluorel 2175) | ketones/esters | ||||
FEX 5832X | 2000 | 200 | 260 | Soluble in | 70.5 |
terpolymer | ketones/esters |
Fluorothermoplastic Terpolymer of Tetrafluoroethylene, |
Hexafluoroproplyene, and |
THV |
220 | 2900 | 600 | 120 | Soluble in | 70.5 |
ketones/ | |||||
Esters (100%) | |||||
|
3480 | 500 | 140 | Soluble in | 71-72 |
ketones/esters | |||||
(partial) | |||||
THV 415 | 4060 | 500 | 155 | Soluble in | 71-72 |
ketones/esters | |||||
(partial) | |||||
|
4060 | 500 | 165 | Soluble in | 72.4 |
ketones/esters | |||||
(partial) | |||||
HTEX 1510 | 4800 | 500 | 165 | Insoluble | 67.0 |
Fluorothermoplastic Copolymer of Tetrafluoroethylene and |
Perfluorovinylether |
PFA | 4350 | 400 | 310 | Insoluble | 76 |
Fluorothermoplastic Copolymer of Tetrafluoroethylene and |
Hexafluoropropylene |
FEP | 2900-4300 | 350 | 260 | Insoluble | 76 |
Fluorothermoplastic Copolymer of Tetrafluoroethylene and Ethylene |
ETFE | 6700 | 325 | 260 | Practically | 61.0 |
insoluble | |||||
TABLE 2 |
High Density Reactive Material Compositions |
Theoretical | ||||||||
Filler | Fluoropolymer | Maximum | ||||||
Metal | Density | Density | Wt % | Wt % | Vol % | Vol % | Density | |
Filler | Fluoropolymer | (g/cm3) | (g/cm3) | Metal | Fluoropolymer | Metal | Fluoropolymer | (g/cm3) |
| THV | 220 | 16.69 | 1.95 | 71.70 | 28.30 | 22.84 | 77.16 | 5.317 |
| THV | 220 | 16.69 | 1.95 | 47.20 | 52.80 | 9.46 | 90.54 | 3.344 |
| THV | 220 | 13.30 | 1.95 | 67.00 | 33.00 | 22.94 | 77.06 | 4.554 |
| THV | 220 | 13.30 | 1.95 | 52.50 | 47.50 | 13.95 | 86.05 | 3.533 |
TABLE 3 |
Safety Data For Ta/ |
Solvent Loss Technique To The Polymer Precipitation Technique |
Thiokol | ABL Sliding | Thiokol | Simulated Bulk | |||
Impact | Friction | ESD | Auto Ignition | DSC Onset | Thiokol | |
Composition | (cm) | (lbs@8 ft/s) | (Joules) | Onset Temp (° F.) | Temp (° C.) | Safety Class |
30.0 |
>46 | 800 | >8.0 | |
435.2 | Green Line- |
70.0% Tantalum | Burned | Safe to | ||||
Solvent Loss | Process | |||||
30.0 |
>46 | 800 | >8.0 | |
360.7 | Green Line- |
70.0% Tantalum | Burned | Safe to | ||||
Polymer Precip. | Process |
30.0 |
ARC Step Heated to 350° C., Ignited |
70.0% Tantalum | |
Solvent Loss | |
30.0 |
ARC: 5 gram sample isothermally aged at 250° C., ignited after 6 hours |
70.0% Tantalum | |
Polymer Precip. | |
-
- 1. Step heat run, 50-580° C., 5° C. steps, 70% Ta/30
% THV 220 Mix #4 (#909), 0.33 grams; - 2. 250° C./24 hour isothermal age run, “isotracked” mode, Ta/
THV 220 1791-64-1, 5.11 grams; - 3. 200° C./24 hour isothermal age run, “isofixed” mode, 70% Ta/30
% THV 220 Solvent Loss 1665-74-1, 1.52 grams; and - 4. 200° C./24 hour isothermal age run, “isofixed” mode, 70% Ta/30
% THV 220 Solvent Loss 1665-74-1, 5.27 grams.
- 1. Step heat run, 50-580° C., 5° C. steps, 70% Ta/30
-
- 1. step heat run, 50-580° C., 5° C. steps, 70% Hf/30
% THV 220 1791-66-1 #1065, 0.31 gram sample; and - 2. 200° C./24 hour isothermal age run, 70% HUf/30
% THV 220 1791-66-1 #1065, 5.16 gram sample.
- 1. step heat run, 50-580° C., 5° C. steps, 70% Hf/30
TABLE 4 |
Ta/ |
Testing Date | Sample Position | Density (g/cc) | % of TMD |
Jan. 21, 2002 | Middle of Rod | 5.256 | 98.86 |
Feb. 4, 2002 | End of Delivered Rod | 5.281 | 99.32 |
Feb. 4, 2002 | Middle of Rod | 5.254 | 98.81 |
Feb. 4, 2002 | Middle of Rod | 5.281 | 99.32 |
Feb. 4, 2002 | End of Delivered Rod | 5.275 | 99.21 |
Average | 5.269 | 99.106 | |
TABLE 5 |
Hf/ |
Testing Date | Sample Position | Density (g/cc) | % of TMD |
Feb. 4, 2002 | End of Delivered Rod | 4.427 | 97.21 |
Feb. 4, 2002 | End of Delivered Rod | 4.440 | 97.49 |
Feb. 4, 2002 | End of Delivered Rod | 4.450 | 97.71 |
Feb. 4, 2002 | End of Delivered Rod | 4.444 | 97.58 |
Average | 4.440 | 97.50 | |
Claims (24)
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US12/507,605 USRE45899E1 (en) | 2000-02-23 | 2009-07-22 | Low temperature, extrudable, high density reactive materials |
US13/372,804 US9103641B2 (en) | 2000-02-23 | 2012-02-14 | Reactive material enhanced projectiles and related methods |
US14/062,635 US20150203415A1 (en) | 2000-02-23 | 2013-10-24 | Reactive material compositions and projectiles including the same |
US14/750,523 US9982981B2 (en) | 2000-02-23 | 2015-06-25 | Articles of ordnance including reactive material enhanced projectiles, and related methods |
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US18431600P | 2000-02-23 | 2000-02-23 | |
US09/789,479 US6593410B2 (en) | 2000-02-23 | 2001-02-21 | High strength reactive materials |
US36828402P | 2002-03-28 | 2002-03-28 | |
US10/386,617 US6962634B2 (en) | 2002-03-28 | 2003-03-12 | Low temperature, extrudable, high density reactive materials |
US55343004P | 2004-03-15 | 2004-03-15 | |
US80194604A | 2004-03-15 | 2004-03-15 | |
US10/801,948 US20050199323A1 (en) | 2004-03-15 | 2004-03-15 | Reactive material enhanced munition compositions and projectiles containing same |
US72346505P | 2005-10-04 | 2005-10-04 | |
US11/538,763 US8122833B2 (en) | 2005-10-04 | 2006-10-04 | Reactive material enhanced projectiles and related methods |
US11/620,205 US8075715B2 (en) | 2004-03-15 | 2007-01-05 | Reactive compositions including metal |
US11/690,016 US7977420B2 (en) | 2000-02-23 | 2007-03-22 | Reactive material compositions, shot shells including reactive materials, and a method of producing same |
US69700507A | 2007-04-05 | 2007-04-05 | |
US12/127,627 US8568541B2 (en) | 2004-03-15 | 2008-05-27 | Reactive material compositions and projectiles containing same |
US12/507,605 USRE45899E1 (en) | 2000-02-23 | 2009-07-22 | Low temperature, extrudable, high density reactive materials |
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