CN111825936A - Aluminum powder/polytetrafluoroethylene composite material and preparation method thereof - Google Patents
Aluminum powder/polytetrafluoroethylene composite material and preparation method thereof Download PDFInfo
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- CN111825936A CN111825936A CN201910308376.1A CN201910308376A CN111825936A CN 111825936 A CN111825936 A CN 111825936A CN 201910308376 A CN201910308376 A CN 201910308376A CN 111825936 A CN111825936 A CN 111825936A
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- 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
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- C08K3/08—Metals
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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
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- C08K3/08—Metals
- C08K2003/0812—Aluminium
Abstract
The invention relates to an aluminum powder/polytetrafluoroethylene composite material and a preparation method thereof, belonging to the technical field of energetic materials, wherein the material consists of 26.5-95% of micron aluminum powder and 5-73.5% of polytetrafluoroethylene, and comprises the following steps: mixing micron aluminum powder, polytetrafluoroethylene and a polar dispersant to form a suspension, adsorbing the polytetrafluoroethylene on the surface of the aluminum powder through intermolecular force, and drying the suspension until the solvent is completely volatilized; in a planet ball mill, through mechanochemical action, Al-F bonding tendency appears between the surfaces of polytetrafluoroethylene and aluminum powder, and the diffusion distance is greatly shortened; and further sintering treatment is carried out, so that the polytetrafluoroethylene is more uniformly distributed on the surface of the aluminum powder. The preparation process of the invention has simple process operation and little environmental pollution, and can implement large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of energetic materials, and particularly relates to an aluminum powder/polytetrafluoroethylene composite material with a core-shell structure and a preparation method thereof.
Background
Fluoropolymers are widely used as coating materials in military fields such as reaction fragments, mixed explosives, pyrotechnic agents and the like. F has strong electronegativity and can perform pre-ignition reaction with an alumina shell layer so as to increase system energy and improve the reaction activity of aluminum, and compared with the traditional formula, the fluorine polymer is used asThe energetic formula of the fuse or the oxidant has higher flame propagation speed, higher flame temperature and more gas production, the fluorine content of Polytetrafluoroethylene (PTFE) is up to 67 percent (molar weight), the friction coefficient is small, the thermal stability is good, the chemical inertness is strong, and the energetic formula can react with alumina to generate CO and AlF3The heat of formation with the monomolecular explosive is less than 12GJ/m3Compared with the aluminum powder/polytetrafluoroethylene (Al/PTFE), the heat of formation of the aluminum powder/polytetrafluoroethylene (Al/PTFE) is up to 21GJ/m3Increasing the total heat release of the system and providing additional energy for further reaction of aluminum, and simultaneously being different from the generation of a compact alumina shell, AlF3The porous structure is dense, a channel is provided for oxygen to enter the aluminum core in the diffusion stage, and the ignition delay phenomenon is improved; further, AlF3Can be sublimated at 1277 ℃, the internal pressure of the system is increased, the particles are crushed, and the agglomeration tendency is reduced, thereby improving the combustion performance.
Aluminum powder/polytetrafluoroethylene composite material is prepared by a ball milling method through Aluminum powder/polytetrafluoroethylene composite material with the advantages of increased specific surface area, reduced initial reaction temperature and capability of reducing agglomeration of gas generated in the reaction process, but the obtained material has uneven particle size distribution due to cold welding effect, and after long-time high-energy extrusion and friction, a sheet structure appears, although the specific surface area is increased, passivation treatment is not carried out in the process, higher potential safety hazard exists, the Aluminum surface is easy to oxidize, the content of active Aluminum is reduced, the enthalpy of combustion is reduced, the flame propagation is hindered due to the existence of large particles, and the combustion efficiency is low under the condition that a strong oxidant is not added; preparation of aluminum powder/polytetrafluoroethylene mechanical activation energetic material and microscopic property research (material report, volume 32, phase 3) of the aluminum powder/polytetrafluoroethylene mechanical activation energetic material, research on preparation of the aluminum powder/polytetrafluoroethylene composite material by high-energy ball milling is carried out, simple characterization is carried out, an exposed surface is generated on the aluminum powder in the process, further oxidation control of the exposed surface is not considered, the microscopic appearance of the aluminum powder is accidentally changed, meanwhile, the aluminum powder and the polytetrafluoroethylene are not uniformly dispersed, the polytetrafluoroethylene cannot form a uniform coating layer on the surface of the aluminum powder, and the microscopic appearance of the obtained composite material is shown in figure 1.
Disclosure of Invention
The invention aims to provide an aluminum powder/polytetrafluoroethylene composite material and a preparation method thereof, and aims to solve the problems of delayed ignition, low combustion rate, insufficient combustion and the like of aluminum powder.
The technical scheme of the invention is as follows: an aluminum powder/polytetrafluoroethylene composite material is composed of 26.5-95% of micron aluminum powder and 5-73.5% of polytetrafluoroethylene.
Further, the composite material is of a core-shell structure, the aluminum powder is used as a core, and the polytetrafluoroethylene is coated on the surface of the aluminum powder.
Further, the average particle size of the aluminum powder is 1-30 mu m.
Further, the average particle size of the polytetrafluoroethylene is 200nm-5 mu m.
The preparation method of the aluminum powder/polytetrafluoroethylene composite material comprises the following steps: (1) weighing aluminum powder and polytetrafluoroethylene according to a proportion, adding a polar dispersant, mixing, and performing ultrasonic oscillation to form a uniform suspension; (2) drying the suspension until the polar dispersant is completely volatilized, transferring the suspension to 50 ℃ for vacuum drying for 2h, and naturally cooling; (3) ball-milling the cooled sample under vacuum, wherein the ball-material ratio is 6:1-12:1, the ball-milling rotation speed is 150r/min-500r/min, and the ball-milling time is 15min-2 h; (5) taking out the ball-milled sample, sintering at 310-340 ℃ in nitrogen atmosphere, preserving heat and naturally cooling; (6) and after sintering, mechanically crushing, sieving and collecting to obtain the composite material.
Further, the polar dispersant is ethanol, acetone or isopropanol.
Further, the volume ratio of the aluminum powder or the polytetrafluoroethylene to the polar dispersant is 1:4-1: 8.
Further, the temperature is increased to 340 ℃ at the speed of 5 k/min-20 k/min for sintering, and the temperature is kept for 2 h.
Compared with the prior art, the invention has the advantages that: 1. the aluminum powder/polytetrafluoroethylene composite material has excellent chemical stability in natural environment, and experiments are carried out in an inert state, so that the obtained composite material is of a well-coated core-shell structure, as shown in figure 2, the composite material is not easy to oxidize in a long-term storage state, and the content of active aluminum is high; 2. the aluminum powder/polytetrafluoroethylene composite material is ignited by the ignition wire in the air atmosphere, the combustion speed is high, the total combustion time of a 100mg sample placed in a conical shape is only about 75ms at the fastest speed, and the method is shown in figure 3; 3. the Al/PTFE composite material is ignited by an ignition wire in the air atmosphere, and a 100mg sample in the closed combustion tank is placed in a conical shape, and the highest pressure reaches 179.15 kPa; 4. the raw materials are cheap, the process operation is simple, the preparation process is safe, the mass industrial production can be realized, and the prospect is wide.
Drawings
FIG. 1 is a scanning electron micrograph of an aluminum powder/polytetrafluoroethylene composite material in the background art.
FIG. 2 is a scanning electron microscope photograph of the aluminum powder/polytetrafluoroethylene composite material obtained by the present invention.
FIG. 3 is a high-speed video recording of the combustion process of the aluminum powder/PTFE composite material obtained by manual mechanical grinding and mixing, taken at a shooting rate of 2000 frames/second in an air atmosphere.
FIG. 4 is a high-speed video recording of the combustion process of the aluminum powder/polytetrafluoroethylene composite material obtained by the present invention in the air atmosphere at a shooting rate of 2000 frames/second.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
6.5g T2 aluminum powder, 3.5g of 200nm PTFE and 80ml of isopropanol are prepared into suspension, the suspension is dried until the isopropanol is completely volatilized, and the powder is collected. Selecting a ball-material ratio of 12:1, setting the rotation speed to be 250r/min, carrying out ball milling for 45min, taking a ball-milled sample 1.5g in a sintering furnace, keeping the temperature for 2h at 340 ℃ in a nitrogen atmosphere, naturally cooling, and collecting the Al/PTFE composite material. Compared with the large-particle block rough structure shown in fig. 1, the Al/PTFE composite material prepared by the invention has uniform particle size distribution, Al and PTFE are well dispersed, and PTFE can be uniformly coated on the surface of aluminum powder to form a core-shell structure, which is shown in fig. 2. The total time for burning of the 100mg samples placed in the cone was only 316 ms. The 100mg sample in the closed combustion can is placed in a cone with the highest pressure of 179.15 kPa.
Under the same proportion, 100mg of the sample obtained after the mixing is only manually ground and placed in a closed combustion can with the highest conical pressure of 141.93 kPa.
Example 2
Taking 7.5g T2 aluminum powder, 2.5g of 200nm PTFE and 50mL of acetone to prepare a suspension, drying until the acetone is completely volatilized, and collecting the powder. Selecting a ball-material ratio of 10:1, setting a rotation speed of 500r/min, performing ball milling for 15min, taking a ball-milled sample 1.5g in a sintering furnace, keeping the temperature for 2h at 340 ℃ in a nitrogen atmosphere, naturally cooling, and collecting the Al/PTFE composite material. The Al/PTFE composite material has good dispersibility, PTFE is uniformly coated on the surface of aluminum powder, and the total combustion time of 100mg samples arranged in a conical shape is only 377 ms; the 100mg sample in the closed combustion can is placed in a cone with the highest pressure of 138.80 kPa.
In the same proportion, the total burning time of the sample obtained after mixing is 443ms under the same condition by only adopting manual grinding.
Example 3
According to the invention, 9.4g T2 aluminum powder, 3.1g of 200nm PTFE and 50mL of acetone are prepared into suspension, the suspension is dried until the acetone is completely volatilized, and the powder is collected. Selecting a ball-material ratio of 8:1, setting the rotation speed to be 250r/min, carrying out ball milling for 60min, taking a ball-milled sample 1.5g in a sintering furnace, carrying out heat preservation for 2h at 325 ℃ in a nitrogen atmosphere, naturally cooling, and collecting the Al/PTFE composite material. The Al/PTFE composite material is found to have good dispersibility, PTFE is uniformly coated on the surface of aluminum powder, and the total combustion time of a sample which is placed in a conical shape and is 100mg is only 391 ms.
In the same proportion, the sample obtained after only manual grinding and mixing is not ignited under the same condition.
Example 4
According to the invention, 14.2g T2 aluminum powder, 2.5g of 200nm PTFE and 90mL of isopropanol are prepared into suspension, the suspension is dried until the isopropanol is completely volatilized, and the powder is collected. Selecting a ball-material ratio of 10:1, setting the rotation speed to be 350r/min, ball milling time to be 15min, taking a ball-milled sample 1.5g in a sintering furnace, keeping the temperature for 2h at 340 ℃ in a nitrogen atmosphere, naturally cooling, and collecting the Al/PTFE composite material. The Al/PTFE composite particles are found to have good dispersibility, PTFE is uniformly distributed on the surface of the aluminum powder, and the total burning time of a sample of which 100mg is arranged in a cone shape is 661 ms.
In the same proportion, the sample obtained after only manual grinding and mixing is not ignited under the same condition.
Example 5
According to the invention, 6.5g of 1-2 mu m aluminum powder, 3.5g of 5 mu m PTFE and 80ml of isopropanol are prepared into a suspension, and the suspension is dried until the isopropanol is completely volatilized, and the powder is collected. Selecting a ball-material ratio of 12:1, setting the rotation speed to be 250r/min, carrying out ball milling for 45min, taking a ball-milled sample 1.5g in a sintering furnace, keeping the temperature for 2h at 340 ℃ in a nitrogen atmosphere, naturally cooling, and collecting the Al/PTFE composite material. The Al/PTFE composite material has good dispersibility, and PTFE is uniformly coated on the surface of aluminum powder. Referring to fig. 4, the burning process was recorded at a high speed in an air atmosphere at a photographing rate of 2000 frames/second, and the total burning time of the sample in a conical shape of 100mg was only 75ms, and it can be seen that the prepared composite material had a shorter ignition delay time and better burning performance.
Fig. 3 is a high-speed video recording of the combustion process of the aluminum powder/polytetrafluoroethylene composite material obtained by only manually grinding and mixing in the same ratio, and shot at a shooting rate of 2000 frames/second in an air atmosphere, wherein the total combustion time of a sample of 100mg placed in a cone shape is about 115 ms.
Claims (8)
1. The aluminum powder/polytetrafluoroethylene composite material is characterized by comprising 26.5-95% of micron aluminum powder and 5-73.5% of polytetrafluoroethylene.
2. The material of claim 1, wherein the composite material is of a core-shell structure, the aluminum powder is a core, and the polytetrafluoroethylene is coated on the surface of the aluminum powder.
3. The material according to claim 1, characterized in that the average particle size of the aluminum powder is 1 μm to 30 μm.
4. The material of claim 1, wherein the mean particle size of the polytetrafluoroethylene is from 200nm to 5 μm.
5. The method for preparing the aluminum powder/polytetrafluoroethylene composite material as claimed in any one of claims 1 to 4, comprising the following steps: (1) weighing aluminum powder and polytetrafluoroethylene according to a proportion, adding a polar dispersant, mixing, and performing ultrasonic oscillation to form a uniform suspension; (2) drying the suspension until the polar dispersant is completely volatilized, transferring the suspension to 50 ℃ for vacuum drying for 2h, and naturally cooling; (3) ball-milling the cooled sample under vacuum, wherein the ball-material ratio is 6:1-12:1, the ball-milling rotation speed is 150r/min-500r/min, and the ball-milling time is 15min-2 h; (5) taking out the ball-milled sample, sintering at 310-340 ℃ in nitrogen atmosphere, preserving heat and naturally cooling; (6) and after sintering, mechanically crushing, sieving and collecting to obtain the composite material.
6. The method of claim 5, wherein the polar dispersant is ethanol, acetone, or isopropanol.
7. The method of claim 5, wherein the volume ratio of the aluminum powder or polytetrafluoroethylene to the polar dispersant is from 1:4 to 1: 8.
8. The method as claimed in claim 5, wherein the temperature is raised to 310-340 ℃ at a rate of 5-20 k/min for sintering, and the temperature is maintained for 2 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114276635A (en) * | 2021-12-13 | 2022-04-05 | 西南科技大学 | Method for preparing high-density aluminum/polytetrafluoroethylene anti-collision composite material |
| CN114833335A (en) * | 2022-04-20 | 2022-08-02 | 西安近代化学研究所 | Coated magnesium powder with combustion micro-explosion effect, preparation method and application thereof |
| CN114989547A (en) * | 2022-06-24 | 2022-09-02 | 佛山科学技术学院 | Polymer composite material with abrasion in-situ repair function and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114276635A (en) * | 2021-12-13 | 2022-04-05 | 西南科技大学 | Method for preparing high-density aluminum/polytetrafluoroethylene anti-collision composite material |
| CN114833335A (en) * | 2022-04-20 | 2022-08-02 | 西安近代化学研究所 | Coated magnesium powder with combustion micro-explosion effect, preparation method and application thereof |
| CN114833335B (en) * | 2022-04-20 | 2023-08-11 | 西安近代化学研究所 | Coated magnesium powder with combustion micro-explosion effect, preparation method and application thereof |
| CN114989547A (en) * | 2022-06-24 | 2022-09-02 | 佛山科学技术学院 | Polymer composite material with abrasion in-situ repair function and preparation method and application thereof |
| CN114989547B (en) * | 2022-06-24 | 2024-01-02 | 佛山科学技术学院 | Polymer composite material with abrasion in-situ repair function and preparation method and application thereof |
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