CN113527018A - Preparation method of Al/PVDF (aluminum/polyvinylidene fluoride) microspheres - Google Patents
Preparation method of Al/PVDF (aluminum/polyvinylidene fluoride) microspheres Download PDFInfo
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- CN113527018A CN113527018A CN202010306469.3A CN202010306469A CN113527018A CN 113527018 A CN113527018 A CN 113527018A CN 202010306469 A CN202010306469 A CN 202010306469A CN 113527018 A CN113527018 A CN 113527018A
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
- C06B33/02—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide with an organic non-explosive or an organic non-thermic component
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- 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
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- 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
- C06B23/001—Fillers, gelling and thickening agents (e.g. fibres), absorbents for nitroglycerine
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Abstract
The invention discloses a preparation method of Al/PVDF microspheres, which is based on an electrostatic spraying principle, adopts nano aluminum powder and PVDF powder as mixed powder to prepare precursor liquid, and the precursor liquid is sprayed and deposited on a substrate at a certain propelling speed under the action of a high-voltage electric field. The Al/PVDF microspheres obtained by the method have the advantages of uniform component distribution, compact combination of Al and PVDF, simple equipment and easy operation, can be used for preparing uniform microspheres in one step, and can be produced at normal temperature and normal pressure without special conditions.
Description
Technical Field
The invention relates to a method for preparing Al/PVDF microspheres, belonging to the field of preparation of energetic materials.
Background
Energetic Materials (EMs) are a class of materials that store large amounts of chemical energy and can be rapidly released, mainly including explosives, pyrotechnical agents and propellants. The nano thermite is a novel energetic material, mainly comprises a nano oxidant and a reducing agent, and generates high temperature and large amount of heat during reaction. However, the nano thermite also has some problems, such as an oxide layer on the surface of the nano aluminum powder and easy agglomeration of the nano aluminum powder, which limits the application of the nano aluminum powder; in order to solve these problems, researchers have conducted a series of studies on the preparation method, material composition, and the like. Wherein the energy density of the fluorine-containing aluminum fuel is higher than that of the aluminum oxygen fuel, and the fluorine-containing aluminum fuel is a high-energy additive in a propellant, an explosive and a priming composition. There are many fluorine-rich polymers such as Polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), Viton, THV, etc. Although PTFE has the highest fluorine content (76 wt.%), it is insoluble in any known solvent, thus limiting its practical application, while PVDF, although having a lower fluorine content (54.9 wt.%), is soluble in some polar solvents and has a low melting point, which establishes its promise for use in nano thermites. PVDF is used as a binder in the preparation process, and Al is uniformly encapsulated in a microsphere; and in the energy release process, PVDF is used as an oxidizing agent to react with Al.
There are many methods for preparing the nano thermite, such as an ultrasonic physical mixing method (prepared samples are easy to agglomerate and are not uniformly dispersed), a sol-gel method (production period is long, operation is complex and impurities are introduced), self-assembly (preparation process is complex, cost is high and yield is low), and the like. These methods all have some defects, and the theory of the electrostatic spraying method is perfect at present, and the method is a simple method for preparing and assembling nano particles, and utilizes the electrostatic field force to disperse and break the molten liquid or liquid solution into tiny droplets. Typically, a higher voltage is applied to the liquid in the tube through a thinner glass or metal tube. Under proper conditions, the liquid will flow out of the tube end and form Taylor cone (Taylor cone), the tail end forms a jet-like thin line and atomization occurs, and the liquid drop is released drop by drop from the tail end of the thin line rapidly, as shown in figure 1. Electrospray produces droplets with a high charge that prevents them from solidifying and promotes their self-dispersion. The size of the liquid drop is very small, and can be reduced to nano level under special condition, and the spray mode can be adjusted by adjusting and controlling the parameters of the liquid flow speed, voltage, the inner diameter of a needle head, the distance between matrixes, the conductivity of the precursor liquid and the like of the electrospray, so as to prepare the monodisperse solid particles with uniform size and adjustable particle size and shape.
Disclosure of Invention
The invention aims to provide a preparation method of Al/PVDF microspheres, which is used for preparing nano thermite microspheres in one step based on an electrostatic spraying method.
The technical solution for realizing the purpose of the invention is as follows:
a preparation method of Al/PVDF microspheres based on an electrostatic spraying principle is based on the electrostatic spraying principle, nano aluminum powder and PVDF powder are used as raw materials, and nano aluminum powder PVDF precursor liquid is sprayed and deposited on a substrate at a certain propelling speed under the action of a high-voltage electric field. The method comprises the following specific steps:
step (1): firstly, adding PVDF powder into a mixed solvent of DMF and acetone, stirring and carrying out ultrasonic treatment until the PVDF powder is fully dissolved to obtain a PVDF solution;
step (2): adding nano aluminum powder into the solution obtained in the step (1), and performing ultrasonic stirring to obtain a mixed powder precursor solution;
and (3): and (3) taking the precursor solution obtained in the step (2) as an electrostatic spraying solution, and obtaining Al/PVDF microsphere powder by adopting an electrostatic spraying process.
Preferably, in step (1), the volume ratio of DMF to acetone is 1: 4.
Preferably, in step (1), the stirring speed is 650-800 rpm, and the stirring time is 2-5 min.
Preferably, in the step (2), the ultrasonic stirring comprises the following specific steps: placing the nano aluminum powder on a magnetic stirrer, stirring the nano aluminum powder for 5 to 10 min at the stirring speed of 650 plus 800 rpm, then ultrasonically treating the nano aluminum powder for 0.5 to 1 h to break the agglomeration among the particles, and then placing the nano aluminum powder on the magnetic stirrer, and stirring the nano aluminum powder for 20 to 24 h at the same speed.
Preferably, in the step (2), the proportion of the PVDF powder in the total mass of the mixed powder (PVDF powder + nano aluminum powder) is 1wt.% to 20 wt.%.
Preferably, in the step (3), the electrostatic spraying process parameters are as follows: the propelling speed is 1.5 mL/h; the high-voltage electric field applied between the needle head and the substrate is 19 (+ -0.25) kV; the distance between the needle and the base was 10 cm.
Compared with the prior art, the Al/PVDF microspheres prepared by the invention have the advantages that:
(1) the invention is based on electrostatic spraying technology, and the micron-sized energetic material with the nanometer characteristic is obtained under the action of a high-voltage electric field. And the obtained Al/PVDF microspheres have uniform distribution of all components and compact combination of Al and PVDF.
(2) The method has simple equipment and easy operation, can prepare uniform microspheres in one step, does not need special conditions, and can produce the microspheres at normal temperature and normal pressure.
Drawings
Fig. 1 is a schematic view of an electrostatic spray process.
FIG. 2 is an SEM image and particle size distribution plot of the Al/PVDF microspheres of example 1.
FIG. 3 is an SEM image and particle size distribution plot of the Al/PVDF microspheres of example 2.
FIG. 4 is an SEM image and particle size distribution plot of the Al/PVDF microspheres of example 3.
FIG. 5 is an EDS map of the Al/PVDF microspheres of example 3.
FIG. 6 is an SEM picture of Al/PVDF from example 4.
FIG. 7 is an XRD analysis of Al/PVDF in examples 1, 2, 3, 4.
Detailed Description
The invention relates to a preparation method of Al/PVDF microspheres, which comprises the following specific steps:
firstly, weighing a proper amount of PVDF, and then dissolving the PVDF in a proper amount of DMF and acetone mixed solvent, wherein the volume ratio of DMF to acetone is 1: 4. Stirring and ultrasonically treating the PVDF to fully dissolve to obtain a PVDF solution, wherein the stirring speed is 650 plus 800 rpm, and stirring is carried out for 2-5 min;
secondly, weighing a proper amount of nano aluminum powder, adding the nano aluminum powder into the PVDF solution, firstly performing magnetic stirring for 5-10 min, then performing ultrasonic treatment for 0.5-1 h to obtain a PVDF dispersion liquid of the nano aluminum powder, and then performing magnetic stirring for 20-24 h to obtain an electrostatic spraying precursor liquid; wherein the stirring speed is 650 plus 800 rpm, the ultrasonic process is to prevent the water temperature in the ultrasonic instrument from being overhigh, the water is changed every 5-10 min, and the water changing time can be properly prolonged in winter;
thirdly, extracting the precursor solution by using a 10 mL injector, placing the precursor solution on an electrostatic spraying instrument (HD-2535, Beijing Yongkang Leye science and technology development Co., Ltd.), adjusting the distance between the aluminum foil substrate and the injector needle to be 10 cm, opening a high-voltage electric field (19 +/-0.25) kV), opening a push injection (speed of 1.5 mL/h) and starting electrostatic spraying, wherein the electrostatic spraying process is shown in figure 1;
and fourthly, stopping injecting after the injection of the precursor liquid in the injector is finished, then closing the electric field, taking down the aluminum foil and scraping the Al/PVDF microsphere powder.
Example 1 was carried out:
first, 6 mg of PVDF powder was weighed and added to 1 mL of DMF: placing the mixture in a solvent with acetone =1:4 (volume ratio) on a magnetic stirrer at 750 rpm, stirring for 2 min, and then carrying out ultrasonic treatment until PVDF is completely dissolved to obtain a PVDF solution;
secondly, weighing 194 mg of nano aluminum powder (the content of active aluminum = 82.1%), adding n-Al into the PVDF solution, firstly placing the PVDF solution on a magnetic stirrer at 650 rpm for stirring for 5 min, then ultrasonically dispersing the PVDF solution for 1 h, and then placing the PVDF solution on the magnetic stirrer at 650 rpm for stirring for 24 h to obtain electrostatic spraying precursor solution;
thirdly, sucking the precursor solution by using a 10 mL injector, placing the precursor solution on an injection of electrostatic spraying, placing an aluminum foil substrate, enabling the distance from a needle to the aluminum foil to be 10 cm, connecting a power supply, enabling the needle to be connected positively, enabling the aluminum foil to be connected negatively, enabling the voltage to be 19 +/-0.25 kV, opening the injection, enabling the speed to be 1.5 mL/h, and starting the electrostatic spraying;
and fourthly, closing the pushing injection and the high-voltage electric field, and taking down the aluminum foil to scrape the product.
Example 2 was carried out:
in the first step, 20mg of PVDF powder is weighed and added to 1 mL of DMF: placing the mixture in a solvent with acetone =1:4 (volume ratio) on a magnetic stirrer at 800 rpm, stirring for 2 min, and then carrying out ultrasonic treatment until PVDF is completely dissolved to obtain a PVDF solution;
secondly, weighing 180 mg of nano aluminum powder (the content of active aluminum = 82.1%), adding n-Al into the PVDF solution, firstly placing the PVDF solution on a magnetic stirrer at 650 rpm for stirring for 5 min, then ultrasonically dispersing the PVDF solution for 1 h, and then placing the PVDF solution on the magnetic stirrer at 650 rpm for stirring for 24 h to obtain electrostatic spraying precursor solution;
thirdly, sucking the precursor solution by using a 10 mL injector, placing the precursor solution on an injection of electrostatic spraying, placing an aluminum foil substrate, enabling the distance from a needle to the aluminum foil to be 10 cm, connecting a power supply, enabling the needle to be connected positively, enabling the aluminum foil to be connected negatively, enabling the voltage to be 19 +/-0.25 kV, opening the injection, enabling the speed to be 1.5 mL/h, and starting the electrostatic spraying;
and fourthly, closing the pushing injection and the high-voltage electric field, and taking down the aluminum foil to scrape the product.
Example 3 of implementation:
in the first step, 30 mg of PVDF powder is weighed and added to 1 mL of DMF: placing the mixture in a solvent with acetone =1:4 (volume ratio) on a magnetic stirrer at 800 rpm, stirring for 4 min, and then carrying out ultrasonic treatment until PVDF is completely dissolved to obtain a PVDF solution;
secondly, weighing 170 mg of nano aluminum powder (the content of active aluminum = 82.1%), adding n-Al into the PVDF solution, firstly placing the PVDF solution on a magnetic stirrer at 650 rpm for stirring for 5 min, then ultrasonically dispersing the PVDF solution for 1 h, and then placing the PVDF solution on the magnetic stirrer at 650 rpm for stirring for 24 h to obtain electrostatic spraying precursor solution;
thirdly, sucking the precursor solution by using a 10 mL injector, placing the precursor solution on an injection of electrostatic spraying, placing an aluminum foil substrate, enabling the distance from a needle to the aluminum foil to be 10 cm, connecting a power supply, enabling the needle to be connected positively, enabling the aluminum foil to be connected negatively, enabling the voltage to be 19 +/-0.25 kV, opening the injection, enabling the speed to be 1.5 mL/h, and starting the electrostatic spraying;
and fourthly, closing the pushing injection and the high-voltage electric field, and taking down the aluminum foil to scrape the product.
Example 4 of implementation:
in the first step, 40 mg of PVDF powder is weighed and added to 1 mL of DMF: placing the mixture in a solvent with acetone =1:4 (volume ratio) on a magnetic stirrer at 800 rpm, stirring for 5 min, and then carrying out ultrasonic treatment until PVDF is completely dissolved to obtain a PVDF solution;
secondly, weighing 160 mg of nano aluminum powder (the content of active aluminum = 82.1%), adding n-Al into the PVDF solution, firstly placing the PVDF solution on a magnetic stirrer at 650 rpm for stirring for 5 min, then ultrasonically dispersing the PVDF solution for 1 h, and then placing the PVDF solution on the magnetic stirrer at 650 rpm for stirring for 24 h to obtain electrostatic spraying precursor solution;
thirdly, sucking the precursor solution by using a 10 mL injector, placing the precursor solution on an injection of electrostatic spraying, placing an aluminum foil substrate, enabling the distance from a needle to the aluminum foil to be 10 cm, connecting a power supply, enabling the needle to be connected positively, enabling the aluminum foil to be connected negatively, enabling the voltage to be 19 +/-0.25 kV, opening the injection, enabling the speed to be 1.5 mL/h, and starting the electrostatic spraying;
and fourthly, closing the pushing injection and the high-voltage electric field, and taking down the aluminum foil to scrape the product.
Characterization test:
FIGS. 2 to 4 are SEM images and particle size distribution diagrams of samples obtained in examples 1 to 3, respectively, and it can be seen that the obtained Al/PVDF microspheres are indeed microspheres, the particle size of the microspheres is between 2 and 5 μm, and the size of the microspheres is slightly increased with the increase of the content of PVDF; as can be seen from the SEM enlarged view, the microspheres are porous structures, and filaments, namely PVDF, are arranged on the surfaces of the microspheres. FIG. 5 is an EDS mapping plot of the sample obtained in example 3, from which it can be seen that the elements F and Al are uniformly distributed, and thus it can be seen that PVDF and Al are uniformly distributed in the microspheres.
FIG. 6 is an SEM image of example 4, comparing the SEM images of examples 1-3, it is clearly observed that the particles are connected by filaments (PVDF), and when the PVDF content reaches 20wt.%, the filaments are significantly increased, and significant PVDF filament connection is seen between the microspheres, and film formation begins.
FIG. 7 is an XRD pattern of the samples of examples 1-4, with Al in the microspheres corresponding to the standard PDF card for Al (PDF # 89-4037), and also illustrates the presence of Al in the microspheres, where no peaks of PVDF are visible, probably because the PVDF content is too low and the diffraction peaks of PVDF are themselves weak.
In conclusion, the invention provides a method for preparing Al/PVDF microspheres, and SEM images and EDS mapping images prove that the method can prepare the Al/PVDF microspheres indeed, and Al and PVDF are uniformly distributed.
Claims (6)
1. A preparation method of Al/PVDF microspheres is characterized in that the method is based on an electrostatic spraying principle, nanometer aluminum powder and PVDF powder are used as mixed powder to prepare precursor liquid, and the precursor liquid is sprayed and deposited on a substrate at a certain propelling speed under the action of a high-voltage electric field, and the method specifically comprises the following steps:
step (1), adding PVDF powder into a mixed solvent of DMF and acetone, stirring and carrying out ultrasonic treatment until the PVDF powder is fully dissolved to obtain a PVDF solution;
step (2), adding nano aluminum powder into the solution obtained in the step (1), and performing ultrasonic stirring to obtain a mixed powder precursor solution;
and (3) taking the precursor liquid obtained in the step (2) as electrostatic spraying liquid, and obtaining Al/PVDF microsphere powder by adopting an electrostatic spraying process.
2. The method of claim 1, wherein in step (1), the volume ratio of DMF to acetone is 1: 4.
3. The method as claimed in claim 1, wherein in the step (1), the stirring speed is 650-800 rpm and the stirring time is 2-5 min.
4. The method of claim 1, wherein in the step (2), the ultrasonic agitation comprises the following specific steps: placing the nano aluminum powder on a magnetic stirrer, stirring the nano aluminum powder for 5 to 10 min at the stirring speed of 650 plus 800 rpm, then ultrasonically treating the nano aluminum powder for 0.5 to 1 h to break the agglomeration among the particles, and then placing the nano aluminum powder on the magnetic stirrer, and stirring the nano aluminum powder for 20 to 24 h at the same speed.
5. The method of claim 1, wherein in step (2), the proportion of PVDF powder in the total mass of the mixed powder is 1wt.% to 20 wt.%.
6. The method of claim 1, wherein in step (3), the electrostatic spray process parameters are as follows: the propelling speed is 1.5 mL/h; the high-voltage electric field applied between the needle head and the substrate is 19 (+ -0.25) kV; the distance between the needle and the base was 10 cm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116063135A (en) * | 2021-10-29 | 2023-05-05 | 南京理工大学 | High-activity composite aluminum powder capable of catalyzing ammonium perchlorate and preparation method thereof |
| CN116354777A (en) * | 2021-12-28 | 2023-06-30 | 南京理工大学 | Electric field controlled explosive granulating method |
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| CN110396033A (en) * | 2019-08-07 | 2019-11-01 | 南京理工大学 | A kind of preparation method of the nanometer thermite based on electrostatic spray |
| CN110452075A (en) * | 2019-07-24 | 2019-11-15 | 西北工业大学 | The preparation method of polymer matrix Composite Energetic Materials coating modification nano-metal particle |
| CN110776384A (en) * | 2019-11-14 | 2020-02-11 | 北京理工大学 | Polymer and nano aluminum powder compounded microsphere |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US9573858B1 (en) * | 2010-03-25 | 2017-02-21 | Energetic Materials Using Amorphous Metals and Metal Alloys | Energetic materials using amorphous metals and metal alloys |
| CN110452075A (en) * | 2019-07-24 | 2019-11-15 | 西北工业大学 | The preparation method of polymer matrix Composite Energetic Materials coating modification nano-metal particle |
| CN110396033A (en) * | 2019-08-07 | 2019-11-01 | 南京理工大学 | A kind of preparation method of the nanometer thermite based on electrostatic spray |
| CN110776384A (en) * | 2019-11-14 | 2020-02-11 | 北京理工大学 | Polymer and nano aluminum powder compounded microsphere |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116063135A (en) * | 2021-10-29 | 2023-05-05 | 南京理工大学 | High-activity composite aluminum powder capable of catalyzing ammonium perchlorate and preparation method thereof |
| CN116354777A (en) * | 2021-12-28 | 2023-06-30 | 南京理工大学 | Electric field controlled explosive granulating method |
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Application publication date: 20211022 |