CN109134171B - Nano-aluminum fluoride high-energy-release fuel - Google Patents
Nano-aluminum fluoride high-energy-release fuel Download PDFInfo
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- CN109134171B CN109134171B CN201811119944.5A CN201811119944A CN109134171B CN 109134171 B CN109134171 B CN 109134171B CN 201811119944 A CN201811119944 A CN 201811119944A CN 109134171 B CN109134171 B CN 109134171B
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
- C06B45/32—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component the coating containing an organic compound
- C06B45/34—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component the coating containing an organic compound the compound being an organic explosive or an organic 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
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
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Abstract
The invention discloses a nano-fluorine-aluminum high-energy-release fuel, and relates to a high-energy-release fuel and a preparation method thereof. The invention aims to solve the problems that the existing preparation method of the fluorine-aluminum composite is more suitable for micron aluminum powder, the thickness of a fluorine-containing shell layer on the surface of the micron aluminum powder is about 100nm, and for nano aluminum powder, the 100nm fluorine-containing shell layer is too thick and heavy to influence the performance of the nano aluminum powder. The nano aluminum fluoride high-energy-release fuel consists of a nano aluminum core and a shell layer, wherein an oxidation film is removed; the method comprises the following steps: firstly, mixing an HF solution with a solvent to obtain a mixed solution; adding nano aluminum powder into the mixed solution, and stirring at normal temperature to obtain a mixed solution containing aluminum powder; adding a perfluorocarboxylic acid solution into the mixed solution containing the aluminum powder, and stirring at normal temperature to obtain a crude product; and fourthly, washing the crude product by using absolute ethyl alcohol, and filtering under reduced pressure to obtain the nano-fluorine-aluminum high-energy-release fuel. The invention is used for preparing the nano-aluminum fluoride high-energy-release fuel.
Description
Technical Field
The invention relates to a high-energy-release fuel and a preparation method thereof.
Background
The solid propellant is an energetic composite material with specific performance, is a power source of various solid engines such as missiles, satellites and the like, and has higher requirements on the performance of the solid propellant along with the development of times and the promotion of space strategic targets. As a novel solid propellant additive, the nano aluminum powder greatly improves the burning rate and the specific impulse, and has no obvious condensation phenomenon in the combustion process, so the nano aluminum powder gradually becomes the current research hotspot. The nano aluminum powder has high surface activity and large specific surface area, so that the storage and preparation of the nano aluminum powder are difficult to a certain degree, the common method for preparing the nano aluminum powder at the present stage is an electric explosion method, namely the surface of an aluminum foil is bombarded by high-voltage electric arc, and simultaneously, a trace amount of oxygen is injected into a system, so that the surface of the aluminum foil has a layer of compact oxide film, but the layer of oxide film does not help a propellant, and meanwhile, the specific surface area is large, the mass ratio is high, so that the practical application of the aluminum foil is limited to a certain degree.
Due to the high enthalpy energy of fluorine and aluminum (Al-F is 664 +/-6 kJ/mol, Al-O is 512 +/-4 kJ/mol), the preparation of novel nano-fluorine-aluminum composite materials is widely researched in recent years. Osborne et al report a polytetrafluoroethylene/aluminum powder composite, suggesting that a "pre-combustion" process occurs between the fluorine-containing surface and the aluminum powder at about 300 ℃ to generate aluminum fluoride and release heat. At present, the preparation methods of the fluorine-aluminum compound are generally two methods: (1) introducing fluorine-containing substances into the metal aluminum powder by mechanical ball milling or physical mixing; (2) through a certain chemical bonding, a layer of fluorine-doped high polymer is coated outside the aluminum powder oxide film. The two methods can not well solve the influence of surface alumina on the performance of the aluminum powder, and are more suitable for micron aluminum powder, the thickness of a fluorine-containing shell layer on the surface of the micron aluminum powder is about 100nm, and for nano aluminum powder, the 100nm fluorine-containing shell layer is too thick and heavy to influence the performance of the nano aluminum powder. Therefore, a layer of uniform fluorine-aluminum composite with a core-shell structure is constructed by a simple method, and the energy release capability of the nano aluminum powder can be greatly improved.
Disclosure of Invention
The invention aims to solve the problems that the existing preparation method of the fluorine-aluminum composite is more suitable for micron aluminum powder, the thickness of a fluorine-containing shell layer on the surface of the micron aluminum powder is about 100nm, and the performance of the nano aluminum powder is influenced because the 100nm fluorine-containing shell layer is too thick, so that the nano fluorine-aluminum high-energy-release fuel and the preparation method thereof are provided.
The nano aluminum fluoride high-energy-release fuel consists of a nano aluminum core and a shell layer, wherein an oxidation film is removed; the nano aluminum core is treated by HF solution to obtain the nano aluminum core without the oxide film, and Al is generated at the same time2F1.5(OH)1.5·0.375H2O aluminium source and Al2F1.5(OH)1.5·0.375H2And the shell is an aluminum perfluorocarboxylate crosslinked network formed by the reaction of an O-aluminum source and perfluorocarboxylic acid.
The preparation method of the nano-fluorine-aluminum high-energy-release fuel comprises the following steps:
firstly, mixing 1-10% of HF solution by mass percent with a solvent to obtain a mixed solution;
the volume ratio of the HF solution with the mass percent of 1-10% to the solvent is 1 (0.5-2);
secondly, adding nano aluminum powder into the mixed solution, and stirring at normal temperature for 3-10 min to obtain a mixed solution containing aluminum powder;
the mass ratio of the volume of the HF solution with the mass percentage of 1-10% in the first step to the mass of the nano aluminum powder in the second step is 10mL (1-3) g;
thirdly, adding a perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L into the mixed solution containing the aluminum powder, and stirring for 2 h-8 h at normal temperature to obtain a crude product;
the solvent in the perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L is the same as the solvent in the first step;
the volume ratio of the mass of the nano aluminum powder in the step two to the volume of the perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L in the step three is 1g (10-20) mL;
and fourthly, washing the crude product by using absolute ethyl alcohol, and filtering under reduced pressure to obtain the nano-fluorine-aluminum high-energy-release fuel.
The invention has the beneficial effects that:
1. the invention relates to a method for establishing a nano-fluorine-aluminum composite structure by directly contacting a high polymer coating layer with an active aluminum core through a perfluorinated carboxylic acid aluminum cross-linked network, which has the following specific reaction mechanism: (1) etching the oxide layer on the surface of the aluminum powder by HF solution, and simultaneously reacting to generate intermediate Al2F1.5(OH)1.5·0.375H2O; (2) intermediate Al2F1.5(OH)1.5·0.375H2Reacting O with a micelle formed by perfluorocarboxylic acid to generate an aluminum perfluorooctanoate micelle; (3) meanwhile, due to the hydrophobic and oleophobic characteristics of the perfluoro aluminum octoate, crosslinking is spontaneously generated to form a final composite structure. The method removes the oxide film on the surface of the nano aluminum powder, and constructs a fluorine-containing shell layer with a thickness similar to that of the nano aluminum powder, and the thickness of the surface coating layer is about 5nmAnd on the right, the oxidation film is basically consistent with the original oxidation film. Wherein, when the perfluorocarboxylic acid is in a proper amount, a perfluorocarboxylic acid coating with the thickness of about 5nm can be constructed, and the coating can be clearly seen as a single layer, and micelles are uniformly arranged on the surface of the aluminum core. The coating layer is too thick, so that the organic coating on the surface of the aluminum powder is too much, the content of active aluminum is reduced, and the total enthalpy value of the aluminum powder is reduced.
2. The nano-fluorine-aluminum high-release energy fuel prepared by the invention shows 154W/g of heat release on the maximum DSC in the first heat release step, and the maximum value of the heat release of the corresponding pure aluminum powder in the first heat release step is 15.5W/g, which is improved by nearly ten times. The perfluorocarboxylic acid coating plays a very critical role, and the organic coating is decomposed at low temperature (150-400 ℃) to enable a layer of extremely thin AlF to appear on the surface of the aluminum powder3And (4) a shell. After the temperature is gradually raised, the shell layer is instantaneously crushed, the oxidation of the whole aluminum powder is completed, and simultaneously, a large amount of heat is discharged.
3. The nano-aluminum fluoride high-energy-release fuel prepared by the method has mild reaction conditions and is suitable for large-scale production.
The invention relates to a nano-aluminum fluoride high-energy-release fuel and a preparation method thereof.
Drawings
FIG. 1 is a TEM image of nano-fluorine aluminum high energy release fuel prepared in example II;
FIG. 2 is a DSC chart, wherein 1 is the nano-aluminum fluoride high-energy-release fuel prepared in example two, and 2 is nano-aluminum powder;
FIG. 3 is an enlarged view of area A in FIG. 2, wherein 1 is the nano-aluminum fluoride high-energy-release fuel prepared in example II, and 2 is nano-aluminum powder;
FIG. 4 is a TG diagram, wherein 1 is the nano-aluminum fluoride high-energy-release fuel prepared in example II, and 2 is nano-aluminum powder;
FIG. 5 is an infrared thermal image of the nano-aluminum fluoride high-energy-release fuel prepared in example II after being ignited for 0 s;
FIG. 6 is an infrared thermal imaging graph of the nano-fluorine aluminum high energy release fuel prepared in the second embodiment when ignited for 0.8 s;
FIG. 7 is an infrared thermal imaging graph of the nano-fluorine aluminum high-energy release fuel prepared in the second embodiment when ignited for 1.44 s;
FIG. 8 is an infrared thermal imaging graph of the nano-fluorine aluminum high-energy release fuel prepared in the second embodiment when ignited for 1.8 s;
FIG. 9 is an infrared thermal imaging graph of the nano-fluorine aluminum high-release energy fuel prepared in the second embodiment when ignited for 2.4 s;
FIG. 10 is an infrared thermal image of the nano-aluminum fluoride high-energy-release fuel prepared in example II after being ignited for 3 s;
FIG. 11 is an infrared thermal imaging graph of the nano aluminum powder when ignited for 0 s;
FIG. 12 is an infrared thermal imaging graph of the nano aluminum powder when ignited for 0.4 s;
FIG. 13 is an infrared thermal imaging graph of the nano-aluminum powder ignited for 0.52 s;
FIG. 14 is an infrared thermal imaging graph of the nano-aluminum powder ignited for 0.92 s;
FIG. 15 is an infrared thermal imaging graph of the nano aluminum powder ignited for 1.32 s;
FIG. 16 is an infrared thermal imaging diagram of the nano aluminum powder ignited for 1.72 s;
fig. 17 is an XRD pattern of the nano-aluminum fluoride high energy release fuel prepared in example two.
Detailed Description
The first embodiment is as follows: the nano-fluorine-aluminum high-energy-release fuel of the embodiment consists of a nano-aluminum core and a shell layer, wherein an oxidation film is removed; the nano aluminum core is treated by HF solution to obtain the nano aluminum core without the oxide film, and Al is generated at the same time2F1.5(OH)1.5·0.375H2O aluminium source and Al2F1.5(OH)1.5·0.375H2And the shell is an aluminum perfluorocarboxylate crosslinked network formed by the reaction of an O-aluminum source and perfluorocarboxylic acid.
The beneficial effects of the embodiment are as follows: 1. the specific embodiment is that a perfluorinated carboxylic acid aluminum cross-linked network establishes a high polymer coating layer which is directly contacted with an active aluminum core to form a nano-fluorine aluminum composite structure, and the specific reaction mechanism is as follows: (1) etching the oxide layer on the surface of the aluminum powder by HF solution, and simultaneously reacting to generate intermediate Al2F1.5(OH)1.5·0.375H2O; (2) intermediate Al2F1.5(OH)1.5·0.375H2Reacting O with micelle formed by perfluorocarboxylic acid to generate perfluorooctanoic acid aluminumClustering; (3) meanwhile, due to the hydrophobic and oleophobic characteristics of the perfluoro aluminum octoate, crosslinking is spontaneously generated to form a final composite structure. The method removes the oxide film on the surface of the nano aluminum powder, and constructs a fluorine-containing shell layer with the thickness similar to that of the nano aluminum powder, wherein the thickness of the surface coating layer is about 5nm and is basically consistent with that of the original oxide film. Wherein, when the perfluorocarboxylic acid is in a proper amount, a perfluorocarboxylic acid coating with the thickness of about 5nm can be constructed, and the coating can be clearly seen as a single layer, and micelles are uniformly arranged on the surface of the aluminum core. The coating layer is too thick, so that the organic coating on the surface of the aluminum powder is too much, the content of active aluminum is reduced, and the total enthalpy value of the aluminum powder is reduced.
2. The nano-fluorine aluminum high-release energy fuel prepared by the embodiment shows 154W/g of heat release on the maximum DSC in the first heat release step, and the heat release maximum of the corresponding pure aluminum powder in the first heat release step is 15.5W/g, which is nearly ten times higher. The perfluorocarboxylic acid coating plays a very critical role, and the organic coating is decomposed at low temperature (150-400 ℃) to enable a layer of extremely thin AlF to appear on the surface of the aluminum powder3And (4) a shell. After the temperature is gradually raised, the shell layer is instantaneously crushed, the oxidation of the whole aluminum powder is completed, and simultaneously, a large amount of heat is discharged.
3. The nano-aluminum fluoride high-energy-release fuel prepared by the specific embodiment has mild reaction conditions and is suitable for large-scale production.
The second embodiment is as follows: the preparation method of the nano-fluorine-aluminum high-energy-release fuel comprises the following steps:
firstly, mixing 1-10% of HF solution by mass percent with a solvent to obtain a mixed solution;
the volume ratio of the HF solution with the mass percent of 1-10% to the solvent is 1 (0.5-2);
secondly, adding nano aluminum powder into the mixed solution, and stirring at normal temperature for 3-10 min to obtain a mixed solution containing aluminum powder;
the mass ratio of the volume of the HF solution with the mass percentage of 1-10% in the first step to the mass of the nano aluminum powder in the second step is 10mL (1-3) g;
thirdly, adding a perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L into the mixed solution containing the aluminum powder, and stirring for 2 h-8 h at normal temperature to obtain a crude product;
the solvent in the perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L is the same as the solvent in the first step;
the volume ratio of the mass of the nano aluminum powder in the step two to the volume of the perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L in the step three is 1g (10-20) mL;
and fourthly, washing the crude product by using absolute ethyl alcohol, and filtering under reduced pressure to obtain the nano-fluorine-aluminum high-energy-release fuel.
The third concrete implementation mode: the second embodiment is different from the first embodiment in that: the solvent in the first step is N, N-dimethylformamide, dimethylacetamide or dimethyl sulfoxide. The rest is the same as the second embodiment.
The fourth concrete implementation mode: this embodiment is different from the second or third embodiment in that: the perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L in the third step is a perfluorodecanoic acid solution with the concentration of 5 g/L-20 g/L, a perfluorooctanoic acid solution with the concentration of 5 g/L-20 g/L or a perfluorobutyric acid solution with the concentration of 5 g/L-20 g/L. The other is the same as the second or third embodiment.
The fifth concrete implementation mode: this embodiment is different from one of the second to fourth embodiments in that: in the first step, 1-5% by mass of HF solution is mixed with a solvent to obtain a mixed solution. The other points are the same as those in the second to fourth embodiments.
The sixth specific implementation mode: the present embodiment is different from one of the second to fifth embodiments in that: and step two, adding nano aluminum powder into the mixed solution, and stirring at normal temperature for 3-5 min to obtain the mixed solution containing the aluminum powder. The other points are the same as those in the second to fifth embodiments.
The seventh embodiment: the present embodiment is different from one of the second to sixth embodiments in that: and in the third step, adding a perfluorocarboxylic acid solution with the concentration of 5 g/L-15 g/L into the mixed solution containing the aluminum powder, and stirring at normal temperature for 2 h-4 h to obtain a crude product. The other points are the same as those in the second to sixth embodiments.
The specific implementation mode is eight: the present embodiment is different from one of the second to seventh embodiments in that: in the first step, 1-2.5% by mass of HF solution is mixed with a solvent to obtain a mixed solution. The other points are the same as those in the second to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the second to eighth embodiments in that: and in the third step, adding a perfluorocarboxylic acid solution with the concentration of 5 g/L-10 g/L into the mixed solution containing the aluminum powder, and stirring at normal temperature for 2 h-5 h to obtain a crude product. The other points are the same as those in the second to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the second to ninth embodiments in that: in the first step, 1-3% by mass of HF solution is mixed with a solvent to obtain a mixed solution. The other points are the same as those in the second to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
the nano aluminum fluoride high-energy-release fuel consists of a nano aluminum core and a shell layer, wherein an oxidation film is removed; the nano aluminum core is treated by HF solution to obtain the nano aluminum core without the oxide film, and Al is generated at the same time2F1.5(OH)1.5·0.375H2O aluminium source and Al2F1.5(OH)1.5·0.375H2The method comprises the following steps of (1) taking an aluminum oxide source and a perfluorocarboxylic acid as a shell layer to form an aluminum perfluorocarboxylate crosslinked network through reaction;
the preparation method of the nano-fluorine-aluminum high-energy-release fuel comprises the following steps:
firstly, mixing an HF solution with the mass percent of 5% with a solvent to obtain a mixed solution;
the solvent is N, N-dimethylformamide;
the volume ratio of the 5% HF solution to the solvent is 1: 2;
adding nano aluminum powder into the mixed solution, and stirring for 5min at normal temperature to obtain a mixed solution containing aluminum powder;
the mass ratio of the volume of the HF solution with the mass percentage of 5% in the first step to the nano aluminum powder in the second step is 10mL:2 g;
thirdly, adding a perfluorodecanoic acid N, N-dimethylformamide solution with the concentration of 15g/L into the mixed solution containing the aluminum powder, and stirring for 4 hours at normal temperature to obtain a crude product;
the volume ratio of the mass of the nano aluminum powder in the step two to the volume of the N, N-dimethylformamide solution of the perfluorodecanoic acid with the concentration of 15g/L in the step three is 1g:20 mL;
and fourthly, washing the crude product by using absolute ethyl alcohol, and filtering under reduced pressure to obtain the nano-fluorine-aluminum high-energy-release fuel.
Example two:
the nano aluminum fluoride high-energy-release fuel consists of a nano aluminum core and a shell layer, wherein an oxidation film is removed; the nano aluminum core is treated by HF solution to obtain the nano aluminum core without the oxide film, and Al is generated at the same time2F1.5(OH)1.5·0.375H2O aluminium source and Al2F1.5(OH)1.5·0.375H2The method comprises the following steps of (1) taking an aluminum oxide source and a perfluorocarboxylic acid as a shell layer to form an aluminum perfluorocarboxylate crosslinked network through reaction;
the preparation method of the nano-fluorine-aluminum high-energy-release fuel comprises the following steps:
firstly, mixing an HF solution with the mass percent of 2.5% with a solvent to obtain a mixed solution;
the solvent is dimethyl sulfoxide;
the volume ratio of the 2.5 percent HF solution to the solvent is 1: 1.3;
adding nano aluminum powder into the mixed solution, and stirring for 5min at normal temperature to obtain a mixed solution containing aluminum powder;
the mass ratio of the volume of the HF solution with the mass percentage of 2.5% in the first step to the nano aluminum powder in the second step is 10mL:1.3 g;
thirdly, adding a dimethyl sulfoxide solution of perfluorooctanoic acid with the concentration of 10g/L into the mixed solution containing the aluminum powder, and stirring for 2 hours at normal temperature to obtain a crude product;
the volume ratio of the mass of the nano aluminum powder in the step two to the volume of the dimethyl sulfoxide solution of the perfluorooctanoic acid with the concentration of 10g/L in the step three is 1g:10 mL;
and fourthly, washing the crude product by using absolute ethyl alcohol, and filtering under reduced pressure to obtain the nano-fluorine-aluminum high-energy-release fuel.
FIG. 1 is a TEM image of nano-fluorine aluminum high energy release fuel prepared in example II; as can be seen from the figure, the thickness of the cladding layer in the nano-fluorine aluminum high-energy-release fuel is about 5 nm.
FIG. 2 is a DSC chart, wherein 1 is the nano-aluminum fluoride high-energy-release fuel prepared in example two, and 2 is nano-aluminum powder; FIG. 3 is an enlarged view of area A in FIG. 2, wherein 1 is the nano-aluminum fluoride high-energy-release fuel prepared in example II, and 2 is nano-aluminum powder; it can be seen from the graph that, compared with the nano aluminum powder, the nano aluminum fluoride high energy release fuel prepared in this example shows an exotherm of 154W/g on the maximum DSC at the first exothermic step, and the corresponding maximum exotherm of the nano aluminum powder is 15.5W/g at the first exothermic step, which is nearly ten times higher, and meanwhile, in the enlarged view, the gas generated during decomposition reacts with the nano aluminum powder to release heat.
FIG. 4 is a TG diagram, wherein 1 is the nano-aluminum fluoride high-energy-release fuel prepared in example II, and 2 is nano-aluminum powder; it can be seen from the figure that the nano-fluorine-aluminum high-release energy fuel prepared by the embodiment is firstly weight-lost and then weight-increased, and the weight-loss corresponds to the decomposition of fluorine-containing substances in the fluorine-aluminum composite material.
FIG. 5 is an infrared thermal image of the nano-aluminum fluoride high-energy-release fuel prepared in example II after being ignited for 0 s; FIG. 6 is an infrared thermal imaging graph of the nano-fluorine aluminum high energy release fuel prepared in the second embodiment when ignited for 0.8 s; FIG. 7 is an infrared thermal imaging graph of the nano-fluorine aluminum high-energy release fuel prepared in the second embodiment when ignited for 1.44 s; FIG. 8 is an infrared thermal imaging graph of the nano-fluorine aluminum high-energy release fuel prepared in the second embodiment when ignited for 1.8 s; FIG. 9 is an infrared thermal imaging graph of the nano-fluorine aluminum high-release energy fuel prepared in the second embodiment when ignited for 2.4 s; FIG. 10 is an infrared thermal image of the nano-aluminum fluoride high-energy-release fuel prepared in example II after being ignited for 3 s;
FIG. 11 is an infrared thermal imaging graph of the nano aluminum powder when ignited for 0 s; FIG. 12 is an infrared thermal imaging graph of the nano aluminum powder when ignited for 0.4 s; FIG. 13 is an infrared thermal imaging graph of the nano-aluminum powder ignited for 0.52 s; FIG. 14 is an infrared thermal imaging graph of the nano-aluminum powder ignited for 0.92 s; FIG. 15 is an infrared thermal imaging graph of the nano aluminum powder ignited for 1.32 s; FIG. 16 is an infrared thermal imaging diagram of the nano aluminum powder ignited for 1.72 s; in conclusion, the ignition temperature of the nano aluminum powder and the nano aluminum fluoride high-energy-release fuel is reduced by comparing the ignition phenomena of the nano aluminum powder and the nano aluminum fluoride high-energy-release fuel, because the ignition temperature is reduced due to the occurrence of the PIR process, the maximum flame temperature of the nano aluminum fluoride high-energy-release fuel reaches 1367 ℃ which is far higher than the flame temperature of the nano aluminum powder in the whole combustion process, and the phenomenon corresponds to the thermogravimetric experiment of the embodiment.
FIG. 17 is an XRD pattern of the nano-aluminum fluoride high energy release fuel prepared in the second embodiment; as can be seen from the figure, the nano aluminum powder itself is not changed, and simultaneously impurity peaks appear at 15.7 degrees, 30.3 degrees, 31.7 degrees, 36.8 degrees, 48.4 degrees and 53.0 degrees (ICSD No.74-0940), and the impurity peaks are analyzed to obtain a nano aluminum core (aluminum oxide) etched by HF, and a byproduct Al obtained by etching the nano aluminum core (aluminum oxide) is obtained2F1.5(OH)1.5·0.375H2And (4) an aluminum O source.
Example three:
the nano aluminum fluoride high-energy-release fuel consists of a nano aluminum core and a shell layer, wherein an oxidation film is removed; the nano aluminum core is treated by HF solution to obtain the nano aluminum core without the oxide film, and Al is generated at the same time2F1.5(OH)1.5·0.375H2O aluminium source and Al2F1.5(OH)1.5·0.375H2The method comprises the following steps of (1) taking an aluminum oxide source and a perfluorocarboxylic acid as a shell layer to form an aluminum perfluorocarboxylate crosslinked network through reaction;
the preparation method of the nano-fluorine-aluminum high-energy-release fuel comprises the following steps:
firstly, mixing an HF solution with the mass percent of 3% with a solvent to obtain a mixed solution;
the solvent is dimethylacetamide;
the volume ratio of the 3% HF solution to the solvent is 1: 1.3;
adding nano aluminum powder into the mixed solution, and stirring for 5min at normal temperature to obtain a mixed solution containing aluminum powder;
the mass ratio of the volume of the HF solution with the mass percentage of 3% in the first step to the nano aluminum powder in the second step is 10mL:1 g;
thirdly, adding a dimethylacetamide solution of perfluorobutyric acid with the concentration of 7g/L into the mixed solution containing the aluminum powder, and stirring for 2 hours at normal temperature to obtain a crude product;
the volume ratio of the mass of the nano aluminum powder in the step two to the dimethylacetamide solution of perfluorobutyric acid with the concentration of 7g/L in the step three is 1g:12 mL;
and fourthly, washing the crude product by using absolute ethyl alcohol, and filtering under reduced pressure to obtain the nano-fluorine-aluminum high-energy-release fuel.
Example four:
the nano aluminum fluoride high-energy-release fuel consists of a nano aluminum core and a shell layer, wherein an oxidation film is removed; the nano aluminum core is treated by HF solution to obtain the nano aluminum core without the oxide film, and Al is generated at the same time2F1.5(OH)1.5·0.375H2O aluminium source and Al2F1.5(OH)1.5·0.375H2The method comprises the following steps of (1) taking an aluminum oxide source and a perfluorocarboxylic acid as a shell layer to form an aluminum perfluorocarboxylate crosslinked network through reaction;
the preparation method of the nano-fluorine-aluminum high-energy-release fuel comprises the following steps:
firstly, mixing an HF solution with the mass percent of 6% with a solvent to obtain a mixed solution;
the solvent is dimethylacetamide;
the volume ratio of the HF solution with the mass percent of 6% to the solvent is 1: 1;
adding nano aluminum powder into the mixed solution, and stirring for 5min at normal temperature to obtain a mixed solution containing aluminum powder;
the mass ratio of the volume of the HF solution with the mass percentage of 6% in the first step to the nano aluminum powder in the second step is 10mL:3 g;
thirdly, adding a dimethylacetamide solution of perfluorobutyric acid with the concentration of 5g/L into the mixed solution containing the aluminum powder, and stirring for 2 hours at normal temperature to obtain a crude product;
the volume ratio of the mass of the nano aluminum powder in the step two to the dimethylacetamide solution of perfluorobutyric acid with the concentration of 5g/L in the step three is 1g:20 mL;
and fourthly, washing the crude product by using absolute ethyl alcohol, and filtering under reduced pressure to obtain the nano-fluorine-aluminum high-energy-release fuel.
Example five:
the nano aluminum fluoride high-energy-release fuel consists of a nano aluminum core and a shell layer, wherein an oxidation film is removed; the nano aluminum core is treated by HF solution to obtain the nano aluminum core without the oxide film, and Al is generated at the same time2F1.5(OH)1.5·0.375H2O aluminium source and Al2F1.5(OH)1.5·0.375H2The method comprises the following steps of (1) taking an aluminum oxide source and a perfluorocarboxylic acid as a shell layer to form an aluminum perfluorocarboxylate crosslinked network through reaction;
the preparation method of the nano-fluorine-aluminum high-energy-release fuel comprises the following steps:
firstly, mixing an HF solution with the mass percent of 5% with a solvent to obtain a mixed solution;
the solvent is N, N-dimethylformamide;
the volume ratio of the 5% HF solution to the solvent is 1: 1.3;
adding nano aluminum powder into the mixed solution, and stirring for 5min at normal temperature to obtain a mixed solution containing aluminum powder;
the mass ratio of the HF solution with the mass percentage of 5% in the first step to the nano aluminum powder in the second step is 10mL:2.5 g;
thirdly, adding an N, N-dimethylformamide solution of perfluorooctanoic acid with the concentration of 6/L into the mixed solution containing the aluminum powder, and stirring for 2 hours at normal temperature to obtain a crude product;
the volume ratio of the mass of the nano aluminum powder in the step two to the volume of the N, N-dimethylformamide solution of the perfluorooctanoic acid with the concentration of 6g/L in the step three is 1g:18 mL;
and fourthly, washing the crude product by using absolute ethyl alcohol, and filtering under reduced pressure to obtain the nano-fluorine-aluminum high-energy-release fuel.
Claims (7)
1. A nanometer aluminum fluoride high energy release fuel is characterized in that the nanometer aluminum fluoride high energy release fuel consists of a nanometer aluminum core and a shell layer, wherein an oxide film is removed; the nano aluminum core is treated by HF solution to obtain the nano aluminum core without the oxide film, and Al is generated at the same time2F1.5(OH)1.5·0.375H2O aluminiumSource, then Al2F1.5(OH)1.5·0.375H2The method comprises the following steps of (1) taking an aluminum oxide source and a perfluorocarboxylic acid as a shell layer to form an aluminum perfluorocarboxylate crosslinked network through reaction;
the preparation method of the nano-fluorine-aluminum high-energy-release fuel comprises the following steps:
firstly, mixing 1-10% of HF solution by mass percent with a solvent to obtain a mixed solution;
the volume ratio of the HF solution with the mass percent of 1-10% to the solvent is 1 (0.5-2);
secondly, adding nano aluminum powder into the mixed solution, and stirring at normal temperature for 3-10 min to obtain a mixed solution containing aluminum powder;
the mass ratio of the volume of the HF solution with the mass percentage of 1-10% in the first step to the mass of the nano aluminum powder in the second step is 10mL (1-3) g;
thirdly, adding a perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L into the mixed solution containing the aluminum powder, and stirring for 2 h-8 h at normal temperature to obtain a crude product;
the solvent in the perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L is the same as the solvent in the first step;
the volume ratio of the mass of the nano aluminum powder in the step two to the volume of the perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L in the step three is 1g (10-20) mL;
fourthly, washing the crude product by using absolute ethyl alcohol and filtering the crude product under reduced pressure to obtain the nano fluorine-aluminum high energy release fuel;
the solvent in the first step is N, N-dimethylformamide, dimethylacetamide or dimethyl sulfoxide;
the perfluorocarboxylic acid solution with the concentration of 5 g/L-20 g/L in the third step is a perfluorodecanoic acid solution with the concentration of 5 g/L-20 g/L, a perfluorooctanoic acid solution with the concentration of 5 g/L-20 g/L or a perfluorobutyric acid solution with the concentration of 5 g/L-20 g/L.
2. The nano-fluorine aluminum high-energy release fuel according to claim 1, characterized in that in the first step, 1-5% by mass of HF solution is mixed with solvent to obtain mixed solution.
3. The nano-fluorine aluminum high-energy release fuel according to claim 1, characterized in that in the second step, nano-aluminum powder is added into the mixed solution, and the mixture is stirred at normal temperature for 3-5 min to obtain the mixed solution containing aluminum powder.
4. The nano-fluorine aluminum high energy release fuel as claimed in claim 1, characterized in that in the third step, a perfluorocarboxylic acid solution with a concentration of 5 g/L-15 g/L is added into the mixed solution containing aluminum powder, and the mixture is stirred for 2 h-4 h at normal temperature to obtain a crude product.
5. The nano-fluorine aluminum high-energy release fuel according to claim 1, characterized in that in the first step, 1-2.5% by weight of HF solution is mixed with solvent to obtain mixed solution.
6. The nano-fluorine aluminum high energy release fuel as claimed in claim 1, characterized in that in the third step, a perfluorocarboxylic acid solution with a concentration of 5 g/L-10 g/L is added into the mixed solution containing aluminum powder, and the mixture is stirred for 2 h-5 h at normal temperature to obtain a crude product.
7. The nano-fluorine aluminum high-energy release fuel according to claim 1, characterized in that in the first step, 1-3% by mass of HF solution is mixed with solvent to obtain mixed solution.
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