CN113649562B - Method for improving dispersibility and reactivity of energetic active material - Google Patents
Method for improving dispersibility and reactivity of energetic active material Download PDFInfo
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- CN113649562B CN113649562B CN202110946814.4A CN202110946814A CN113649562B CN 113649562 B CN113649562 B CN 113649562B CN 202110946814 A CN202110946814 A CN 202110946814A CN 113649562 B CN113649562 B CN 113649562B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
Abstract
The invention discloses a method for improving the flowability and reactivity of an energy-containing active material, which comprises the following steps: the method comprises the following steps: a double-planetary power stirrer is adopted, and a low-speed stirring paddle and a sawtooth-shaped dispersion disc arranged on a high-speed dispersion shaft rotate and revolve; step two: the low-speed stirring paddle generates strong kneading interference motion and up-down/left-right circulating motion for the materials by combining the low-clearance design of the stirring paddle; step three: the high-speed dispersion disc intensively shears and breaks up the materials, so that the materials are finally ensured to be fully dispersed and uniformly blended and mixed; the invention further improves the power of fragment penetration and explosion and the capacity of batch production.
Description
Technical Field
The invention relates to the field of active fragment materials, in particular to a method for improving the flowability and reactivity of an energy-containing active material.
Background
The metal/fluoropolymer energetic active material is called as 'impact-initiated reaction material', is formed by pressing and sintering two or more non-explosive solids, is very insensitive and safe in a static state, has certain toughness and strength, can be directly machined, and generates violent explosion and combustion under the action of high-speed impact to generate high heat and high temperature; the active fragments prepared by the method can comprehensively damage air targets such as cruise missiles, ballistic missiles, fighters and the like by using high kinetic energy and high chemical energy released after impact explosion, so that the damage effect is greatly improved.
The metal/fluoropolymer energetic active material mostly takes aluminum powder and polytetrafluoroethylene (Al/PTFE) as main components, and the density and the strength are low, so that the damage effect is influenced. In order to improve and overcome these problems and to increase the penetration and explosion power, patent CN105348704A proposes to add heavy metal tungsten powder to the composition, and when the mass fraction of W is 60%, the density can reach 3.88g/cm3The dynamic strength limit can reach 119.3 MPa. However, the addition of large amounts of inert metal prevents sufficient contact between the active metal and the polytetrafluoroethylene component, affecting the energy density and extent of reaction of the energetic active material. Meanwhile, the metal/fluoropolymer energetic active material matrix is generally selected from suspended polytetrafluoroethylene fine particle resin, and the properties such as filling strength of metal particles are improved to a certain extent, but because the compatibility with the matrix is poor, the affinity is small, an obvious interface appears in the matrix, and the dispersion is not easy to be uniform, the mechanical strength of the broken piece is not enough, and the reaction degree is also influenced. In addition, the energetic active material obtained by simple mixing, in addition to being non-uniform in dispersion, is also poorly flowable and difficult to use in mass production, which is also a metalThe application of the fluoropolymer energetic active material must be considered.
Disclosure of Invention
The invention aims to improve the strength, the reaction degree and the powder flowability of the existing metal/fluoropolymer energetic active material, further improve the power of fragment penetration and explosion and the capacity of batch production, and provides a method for improving the flowability and the reactivity of the energetic active material.
The present invention relates to a method for improving the flowability and reactivity of energetic active materials,
a method of improving the dispersibility and reactivity of an energetic active material comprising the steps of:
the method comprises the following steps: a double-planetary power stirrer is adopted, and a low-speed stirring paddle and a sawtooth-shaped dispersion disc arranged on a high-speed dispersion shaft rotate and revolve;
step two: meanwhile, the low-speed stirring paddle is combined with the low-clearance design of the stirring paddle, so that the materials generate strong kneading interference motion and up-down/left-right circulating motion;
step three: the high-speed dispersion disc intensively shears and breaks up the materials; thereby finally ensuring that the materials are fully dispersed and uniformly blended (mixed).
Preferably, the energy-containing active material prepared by the method takes aluminum powder/magnesium powder/suspended polytetrafluoroethylene powder/tungsten powder as a main component, and polytetrafluoroethylene superfine powder, nano-scale alumina powder and graphite are added as auxiliary components, so that the energy-containing active material has the characteristics and advantages of uniform powder dispersion, good free-running property, convenience for batch preparation, high fragment strength, high reaction degree, safety, insensitivity and the like, and can be widely applied to the field of air defense and reverse conduction.
Wherein the polytetrafluoroethylene superfine powder is processed by a special process, and the average particle size of the polytetrafluoroethylene superfine powder is 2-3 microns. The polytetrafluoroethylene not only keeps the inherent excellent characteristics of polytetrafluoroethylene such as chemical resistance, thermal stability, weather resistance, temperature resistance and the like, but also has a plurality of unique properties such as larger specific surface area, good dispersibility, self-lubricity and the like. Therefore, it can be used as a solid lubricantCan also be used as an active component to participate in the reaction. The nano-alumina can perform a pre-ignition reaction with the polytetrafluoroethylene, so Al is used2O3As an additive, Al2O3As an excellent ceramic material, the material has extremely high hardness, and the mechanical property of the active material can be enhanced while the energy density of the active material is improved.
The purpose of the invention is realized by the following technical scheme.
A method for improving the flowability and reactivity of energetic active materials comprises the following specific steps:
the method comprises the following steps: placing aluminum powder, magnesium powder, tungsten powder, polytetrafluoroethylene superfine powder, nano aluminum oxide and graphite in a double-planet power stirrer for preliminary mixing; wherein, 5-15 parts of aluminum powder with the particle size of 10-75 μm; 5-15 parts of magnesium powder with the particle size of 10-75 mu m; 30-60 parts of tungsten powder, and the particle size is 1-75 mu m; 0.1-5 parts of polytetrafluoroethylene superfine powder with the particle size of 2-3 mu m; 1-5 parts of nano aluminum oxide with the particle size of 10-200 nm; 0.1-1 part of graphite with the particle size of 1-38 mu m;
step two: placing the uniformly mixed powder and the suspended polytetrafluoroethylene powder in a double-planet power stirrer for secondary mixing; wherein, 30-60 parts of polytetrafluoroethylene powder with the particle size of 60-160 mu m;
step three: placing the mixed powder obtained in the step two in a custom mold, and performing compression molding to obtain a molded piece;
step four: and sintering the molded piece obtained in the third step to obtain a final test piece.
Preferably, the mixing time in the first step and the second step is 1-6h, the speed of the stirring paddle is 0-53rpm, and the dispersion rotating speed is 0-1000 rpm.
Preferably, the pressing pressure in the third step is 10-50MPa, and the pressure maintaining time is 5-10 min.
Preferably, the sintering temperature in the fourth step is 350-380 ℃, and the sintering time is 1-2 h.
Advantageous effects
1. The invention adopts the conventional aluminum powder, magnesium powder, tungsten powder and polytetrafluoroethylene powder as main raw materials, has wide sources and low price;
2. the invention adopts a double-planetary power stirrer to carry out primary mixing, secondary mixing, die pressing and sintering processes, has simple process, no special process requirement, low cost and convenient batch production.
3. The energetic active material powder prepared by the invention has uniform dispersion and good free-running property, and is convenient for large-scale batch production.
4. The active fragment prepared from the energy-containing active material has good formability, further improves the mechanical strength, and greatly improves the energy density and the reaction degree.
5. The invention is tested in the target range, the penetration and explosion power is obviously improved, and the invention can ignite or detonate the cotton quilt or the aluminum oil tank filled with RP-3 aviation kerosene after the double-layer spacing target '6 mmQ235 steel plate and 2mmLY12 aluminum plate'.
Drawings
FIG. 1 is a photograph of the combined effect of active fragments prepared from energetic active materials on a double layer spacer target and a quilt behind the target;
FIG. 2 is a photograph showing the combined effects of active fragments prepared from energetic active materials on fuel tanks after 6mm Q235 steel plates and targets;
fig. 3 is a flow chart of the method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, which are not intended to limit the present invention in any manner. Unless otherwise indicated, the various starting materials used in the examples of the present invention are either conventionally available commercially or prepared according to conventional methods in the art using equipment commonly used in the laboratory. Unless defined or stated otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
A method for improving the flowability and reactivity of energetic active materials comprises the following specific steps:
preliminary mixing: weighing 10 parts of aluminum powder, 55 parts of tungsten powder, 5 parts of polytetrafluoroethylene superfine powder, 5 parts of nano aluminum oxide and 0.5 part of graphite, placing the materials into a double-planetary power mixer for preliminary mixing, and drying for 6 hours at the mixing paddle speed of 50rpm, the dispersion rotating speed of 1000rpm and the drying temperature of 60 ℃; wherein the particle size of the aluminum powder is 10 mu m, the particle size of the tungsten powder is 10 mu m, the particle size of the polytetrafluoroethylene ultrafine powder is 2 mu m, the particle size of the nano aluminum oxide is 20nm, and the particle size of the graphite is 1 mu m;
and (3) secondary mixing: placing the uniformly mixed powder and 25 parts of suspended polytetrafluoroethylene powder into a double-planetary power mixer for secondary mixing and drying, wherein the mixing time is 6 hours, the stirring paddle speed is 50rpm, the dispersion rotating speed is 1000rpm, and the drying temperature is 60 ℃; wherein, the particle size of the polytetrafluoroethylene powder is 60 μm;
pressing: weighing a certain mass of powder according to the theoretical density of the mixed powder and the volume of a test piece, adding the powder into a mold cavity at one time, performing compression molding under the compression pressure of 30MPa and the pressure maintaining time of 5min, demolding to obtain a blank, and standing for 24h at room temperature;
and (3) sintering: and placing the parison in a furnace chamber of a vacuum sintering furnace, and filling argon. Sintering and molding at the sintering temperature of 380 ℃, the sintering time of 2h, the heat preservation temperature of 327 ℃, the heat preservation time of 2h and the temperature rise and fall rate of 1 ℃/min to obtain the final test piece.
Compared with the conventional Al/PTFE/W active fragment, the final test piece obtained in the embodiment has the advantages that the mechanical strength is remarkably improved, the dynamic ultimate strength can reach 148.23MPa, the reaction degree is improved, and the damage effect is remarkably improved.
Example 2
A method for improving the flowability and reactivity of energetic active materials comprises the following specific steps:
preliminary mixing: weighing 10 parts of aluminum powder, 5 parts of magnesium powder, 50 parts of tungsten powder, 10 parts of polytetrafluoroethylene superfine powder, 5 parts of nano aluminum oxide and 0.5 part of graphite, placing the mixture in a double-planet power stirrer for preliminary mixing, and drying for 6 hours, wherein the stirring paddle speed is 50rpm, the dispersion rotating speed is 1000rpm, and the drying temperature is 60 ℃; wherein the particle size of the aluminum powder is 10 mu m, the particle size of the magnesium powder is 10 mu m, the particle size of the tungsten powder is 10 mu m, the particle size of the polytetrafluoroethylene ultrafine powder is 2 mu m, the particle size of the nano aluminum oxide is 20nm, and the particle size of the graphite is 1 mu m;
and (3) secondary mixing: placing the uniformly mixed powder and 20 parts of suspended polytetrafluoroethylene powder into a double-planetary power mixer for secondary mixing and drying, wherein the mixing time is 6 hours, the stirring paddle speed is 50rpm, the dispersion rotating speed is 1000rpm, and the drying temperature is 60 ℃; wherein, the particle size of the polytetrafluoroethylene powder is 60 μm;
pressing: weighing a certain mass of powder according to the theoretical density of the mixed powder and the volume of a test piece, adding the powder into a mold cavity at one time, performing compression molding under the compression pressure of 30MPa and the pressure maintaining time of 5min, demolding to obtain a blank, and standing for 24h at room temperature;
and (3) sintering: and placing the parison in a furnace chamber of a vacuum sintering furnace, and filling argon. Sintering and molding at the sintering temperature of 380 ℃, the sintering time of 2h, the heat preservation temperature of 327 ℃, the heat preservation time of 2h and the temperature rise and fall rate of 1 ℃/min to obtain the final test piece.
Compared with the conventional Al/PTFE/W active fragment, the mechanical strength of the final test piece obtained in the embodiment is improved, the dynamic ultimate strength can reach 124.80MPa, and due to the addition of magnesium powder, the energy density and the reaction degree are greatly improved, and the damage effect is obviously improved.
Example 3
A method for improving the flowability and reactivity of energetic active materials comprises the following specific steps:
preliminary mixing: weighing 10 parts of aluminum powder, 50 parts of tungsten powder, 10 parts of polytetrafluoroethylene superfine powder, 10 parts of nano aluminum oxide and 0.1 part of graphite, placing the materials into a double-planetary power mixer for preliminary mixing, and drying for 6 hours at a stirring paddle speed of 50rpm, a dispersion rotating speed of 500rpm and a drying temperature of 60 ℃; wherein the particle size of the aluminum powder is 10 mu m, the particle size of the tungsten powder is 1 mu m, the particle size of the polytetrafluoroethylene ultrafine powder is 2 mu m, the particle size of the nano aluminum oxide is 10nm, and the particle size of the graphite is 1 mu m;
and (3) secondary mixing: placing the uniformly mixed powder and 20 parts of suspended polytetrafluoroethylene powder into a double-planetary power mixer for secondary mixing and drying, wherein the mixing time is 6 hours, the stirring paddle speed is 50rpm, the dispersion rotating speed is 500rpm, and the drying temperature is 60 ℃; wherein, the particle size of the polytetrafluoroethylene powder is 60 μm;
pressing: weighing a certain mass of powder according to the theoretical density of the mixed powder and the volume of a test piece, adding the powder into a mold cavity at one time, performing compression molding under the compression pressure of 30MPa and the pressure maintaining time of 5min, demolding to obtain a blank, and standing for 24h at room temperature;
and (3) sintering: and placing the parison in a furnace chamber of a vacuum sintering furnace, and filling argon. And sintering and molding at the sintering temperature of 360 ℃, the sintering time of 2h, the heat preservation temperature of 327 ℃, the heat preservation time of 2h and the temperature rise and fall rate of 1 ℃/min to obtain the final test piece.
Compared with the conventional Al/PTFE/W active fragment, the mechanical strength of the final test piece obtained in the embodiment is greatly improved, the dynamic ultimate strength can reach 135.67MPa, and due to the addition of the polytetrafluoroethylene ultrafine powder and the nano alumina, the reaction degree is obviously improved, and the damage effect is obviously improved.
Example 4
A method for improving the flowability and reactivity of energetic active materials comprises the following specific steps:
preliminary mixing: weighing 5 parts of aluminum powder, 10 parts of magnesium powder, 45 parts of tungsten powder, 10 parts of polytetrafluoroethylene superfine powder and 10 parts of nano aluminum oxide, placing the materials into a double-planet power stirrer for preliminary mixing, and drying for 6 hours at a stirring paddle speed of 50rpm, a dispersion rotating speed of 500rpm and a drying temperature of 60 ℃; wherein the particle size of the aluminum powder is 10 mu m, the particle size of the magnesium powder is 10 mu m, the particle size of the tungsten powder is 1 mu m, the particle size of the polytetrafluoroethylene ultrafine powder is 2 mu m, the particle size of the nano aluminum oxide is 10nm, and the particle size of the graphite is 1 mu m;
and (3) secondary mixing: placing the uniformly mixed powder and 20 parts of suspended polytetrafluoroethylene powder into a double-planetary power mixer for secondary mixing and drying, wherein the mixing time is 6 hours, the stirring paddle speed is 50rpm, the dispersion rotating speed is 500rpm, and the drying temperature is 60 ℃; wherein, the particle size of the polytetrafluoroethylene powder is 60 μm;
pressing: weighing a certain mass of powder according to the theoretical density of the mixed powder and the volume of a test piece, adding the powder into a mold cavity at one time, performing compression molding under the compression pressure of 30MPa and the pressure maintaining time of 5min, demolding to obtain a blank, and standing for 24h at room temperature;
and (3) sintering: and placing the parison in a furnace chamber of a vacuum sintering furnace, and filling argon. Sintering and molding at the sintering temperature of 380 ℃, the sintering time of 1h, the heat preservation temperature of 327 ℃, the heat preservation time of 2h and the temperature rise and fall rate of 1 ℃/min to obtain the final test piece.
Compared with the conventional Al/PTFE/W active fragment, the mechanical strength of the final test piece obtained in the embodiment is remarkably improved, the dynamic ultimate strength can reach 145.47MPa, and due to the addition of the magnesium powder, the polytetrafluoroethylene superfine powder and the nano alumina, the energy density and the reaction degree are greatly improved, and the damage effect is remarkably improved.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A method for improving the dispersibility and reactivity of an energetic active material, comprising the steps of:
the method comprises the following steps: placing aluminum powder, magnesium powder, tungsten powder, polytetrafluoroethylene superfine powder, nano aluminum oxide and graphite in a double-planetary power mixer for preliminary mixing, wherein a double-planetary power mixer is adopted, and a low-speed stirring paddle and a serrated dispersion disc arranged on a high-speed dispersion shaft rotate and revolve; the low-speed stirring paddle generates strong kneading interference motion and up-down/left-right circulating motion for the materials by combining the low-clearance design of the stirring paddle;
the high-speed dispersion disc intensively shears and breaks up the materials, so that the materials are finally ensured to be fully dispersed and uniformly blended and mixed;
step two: placing the uniformly mixed powder and the suspended polytetrafluoroethylene powder in a double-planet power stirrer for secondary mixing;
step three: placing the mixed powder obtained in the step two in a custom mold, and performing compression molding to obtain a molded piece;
step four: and sintering the molded piece obtained in the third step to obtain a final test piece.
2. The method of improving the flowability and reactivity of an energetic active material according to claim 1, wherein: the energetic active material comprises the following components in parts by weight: wherein, the aluminum powder is 5 to 15 parts, and the particle size is 10 to 75 mu m; 5-15 parts of magnesium powder with the particle size of 10-75 mu m; 30-60 parts of tungsten powder with the particle size of 1-75 mu m; 30-60 parts of suspended polytetrafluoroethylene powder with the particle size of 60-160 mu m; 0.1-5 parts of polytetrafluoroethylene superfine powder with the particle size of 2-3 mu m; 1-5 parts of nano aluminum oxide with the particle size of 10-200 nm; 0.1-1 part of graphite with the grain diameter of 1-38 mu m.
3. The method of improving the flowability and reactivity of an energetic active material according to claim 1, wherein: the mixing time in the first step and the second step is 1-6h, the speed of a stirring paddle is 0-53rpm, and the dispersion rotating speed is 0-1000 rpm.
4. The method of improving the flowability and reactivity of an energetic active material according to claim 1, wherein: and step three, the pressing pressure is 10-50MPa, and the pressure maintaining time is 5-10 min.
5. The method of improving the flowability and reactivity of an energetic active material according to claim 1, wherein: and fourthly, the sintering temperature is 350-380 ℃, and the sintering time is 1-2 h.
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Inventor after: Shu Qinghai Inventor after: Jiang Yuexian Inventor after: Zhao Shuai Inventor after: Lv Xijuan Inventor after: Cheng Lirong Inventor after: Shi Yansong Inventor after: Wang Dongxu Inventor after: Zou Haoming Inventor after: Xu Bolin Inventor after: Wen Ping Inventor before: Shu Qinghai Inventor before: Jiang Yuexian Inventor before: Zhao Shuai Inventor before: Lv Xijuan Inventor before: Cheng Lirong Inventor before: Shi Yansong Inventor before: Wang Dongxu Inventor before: Zou Haoming Inventor before: Xu Bolin Inventor before: Wen Ping |