CN109134171A - A kind of nanometer of fluorine aluminium height releases energy fuel and preparation method thereof - Google Patents
A kind of nanometer of fluorine aluminium height releases energy fuel and preparation method thereof Download PDFInfo
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- CN109134171A CN109134171A CN201811119944.5A CN201811119944A CN109134171A CN 109134171 A CN109134171 A CN 109134171A CN 201811119944 A CN201811119944 A CN 201811119944A CN 109134171 A CN109134171 A CN 109134171A
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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
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
Abstract
A kind of nanometer of fluorine aluminium height release can fuel and preparation method thereof, the present invention relates to a kind of high release can fuel and preparation method thereof.The problem of the invention solves the preparation methods of existing fluorine aluminium compound to be more suitable for a micron aluminium powder, and micron aluminium powder fluorine-contained surface shell thickness is in 100nm or so, and for nanometer aluminium powder, the fluorine-containing shell of 100nm is excessively thick and heavy, influences its performance.Nanometer fluorine aluminium height is released energy fuel and is made of the nanometer aluminium core and shell for removing oxide film dissolving；Method: one, HF solution with solvent is mixed, obtains mixed solution；Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature obtains the mixed solution containing aluminium powder；Three, perfluorocarboxylic acid solution is added into the mixed solution containing aluminium powder, stirring at normal temperature obtains crude product；Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.The present invention releases the preparation of energy fuel for nanometer fluorine aluminium height.
Description
Technical field
The present invention relates to a kind of high release can fuel and preparation method thereof.
Background technique
Solid propellant is a kind of composite material containing energy of particular characteristic, is all kinds of solid engines such as guided missile, satellite
Power source, with the development of the times, the promotion of aerospace strategy target, to the performance of solid propellant, more stringent requirements are proposed.
Nanometer aluminium powder greatly improves its burn rate, specific impulse, and in combustion as a kind of novel solids flux
Without obvious coacervation, therefore, nanometer aluminium powder is increasingly becoming current research hot spot.Nanometer aluminium powder high surface activity, specific surface area
Greatly, therefore all there is certain difficulty in its storage and preparation, and the method for commonly preparing nanometer aluminium powder at this stage is blasting, i.e., logical
High-voltage arc bombardment aluminium foil surface is crossed, while injecting trace oxygen in system, makes its surface that there is one layer of fine and close oxidation film, but
This layer oxide film has no help to propellant, simultaneously because large specific surface area, quality accounts for relatively high, results in it and is actually answering
Certain restrictions is received in.
Due to the high enthalpy of fluorine and aluminium energy (Al-F is that 664 ± 6kJ/mol, Al-O are 512 ± 4kJ/mol), Performances of Novel Nano-Porous is prepared
Rice fluorine aluminium composite material is widely studied in recent years.Osborne et al. reports polytetrafluoroethylene (PTFE)/aluminium powder compound, mentions
Fluorochemical surface and aluminium powder will appear " precombustion " process at 300 DEG C or so out, generate aluminum fluoride and discharge heat simultaneously.Existing rank
There are two types of the preparation method of section fluorine aluminium compound is usual: (1) introducing and contain in metallic aluminium powder by mechanical ball mill or physical mixed
Fluorine material；(2) by being centainly chemically bonded, in one layer of fluorine doped high polymer of aluminium powder oxidation film outer cladding.This both of which cannot
Surface alumina oxide is solved very well in the presence of the influence to aluminium powder performance, while this two kinds of methods are more suitable for a micron aluminium powder, it is micro-
Rice aluminium powder fluorine-contained surface shell thickness is in 100nm or so, and for nanometer aluminium powder, the fluorine-containing shell of 100nm is excessively thick and heavy, instead
And influence its performance.Therefore the fluorine aluminium compound of one layer of uniform core-shell structure, and energy are constructed by a kind of simple method
The energy releasability of significant increase nanometer aluminium powder is current research hot spot.
Summary of the invention
The invention solves the preparation methods of existing fluorine aluminium compound to be more suitable for a micron aluminium powder, micron aluminium powder surface
Fluorine-containing shell thickness is in 100nm or so, and for nanometer aluminium powder, the fluorine-containing shell of 100nm is excessively thick and heavy, influences its performance
Problem, thus a kind of nanometer of fluorine aluminium height is provided and releases energy fuel and preparation method thereof.
Nanometer fluorine aluminium height is released energy fuel and is made of the nanometer aluminium core and shell for removing oxide film dissolving；HF solution handles nanometer aluminium core
The nanometer aluminium core of oxide film dissolving is obtained, while generating Al2F1.5(OH)1.5·0.375H2O silicon source, then with Al2F1.5(OH)1.5·
0.375H2O silicon source and perfluorocarboxylic acid react the aluminium cross-linked network of the perfluorocarboxylic acid to be formed as shell.
The preparation method that a kind of nanometer of fluorine aluminium height releases energy fuel is to sequentially include the following steps:
One, the HF solution that mass percent is 1%~10% is mixed with solvent, obtains mixed solution；
The volume ratio of HF solution and solvent that the mass percent is 1%~10% is 1:(0.5~2)；
Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature 3min~10min obtains the mixed solution containing aluminium powder；
Nanometer described in the volume and step 2 of the HF solution that mass percent described in step 1 is 1%~10%
The mass ratio of aluminium powder is 10mL:(1~3) g；
Three, the perfluorocarboxylic acid solution that concentration is 5g/L~20g/L, stirring at normal temperature 2h are added into the mixed solution containing aluminium powder
~8h, obtains crude product；
The concentration is that solvent is identical as solvent described in step 1 in the perfluorocarboxylic acid solution of 5g/L~20g/L；
Concentration described in the quality and step 3 of nanometer aluminium powder described in step 2 is the perfluor carboxylic of 5g/L~20g/L
The volume ratio of acid solution is 1g:(10~20) mL；
Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.
The beneficial effects of the present invention are:
1, the present invention establishes class high polymer clad for a kind of aluminium cross-linked network of perfluorocarboxylic acid and directly contacts with active aluminium core
Nanometer fluorine aluminum compound structure is formed, specific the reaction mechanism is as follows: (1) oxide layer on HF solution etches aluminium powder surface, simultaneous reactions
Generate intermediate A l2F1.5(OH)1.5·0.375H2O；(2) intermediate A l2F1.5(OH)1.5·0.375H2O and perfluorocarboxylic acid institute shape
At micelle carry out reaction generate perfluoro caprylic acid aluminium group；(3) while perfluoro caprylic acid aluminium is due to the spontaneous production of the characteristic of its hydrophobic oleophobic
Raw crosslinking, forms final composite construction.While this method removes nanometer aluminium powder surface film oxide, one layer and its thickness are constructed
Similar fluorine-containing shell, surface coating layer thickness are almost the same compared with former oxidation film in 5nm or so.Wherein, work as perfluorocarboxylic acid
The perfluorocarboxylic acid coating of 5nm or so can be constructed when appropriate, and coating can be clearly seen as single layer at this time, micelle is on aluminium core surface
Evenly distributed generation.Clad is blocked up, and it is excessive to will lead to aluminium powder surface organic coating, and active aluminium content decline reduces its total enthalpy
Value.
2, nanometer fluorine aluminium height prepared by the present invention releases energy fuel and shows that heat release is on maximum DSC in the first heat release step
154W/g, and corresponding to pure aluminium powder in the first heat release step heat release maximum value is 15.5W/g, nearly ten times of promotion occurs.At this
In perfluorocarboxylic acid clad play extremely critical effect, organic coating decomposes (150 DEG C -400 DEG C) at low temperature and makes aluminium
There is one layer of very thin AlF in powder surface3Shell.After being gradually warmed up, the shell moment is broken, and oxidation is completed inside entire aluminium powder,
Big calorimetric is released simultaneously.
3, nanometer fluorine aluminium height prepared by the present invention releases energy fuel, and reaction condition is mild, is suitable for fairly large production.
The present invention releases energy fuel and preparation method thereof for a kind of nanometer of fluorine aluminium height.
Detailed description of the invention
Fig. 1 is the TEM figure that nanometer fluorine aluminium height prepared by embodiment two releases energy fuel；
Fig. 2 is DSC figure, and 1 releases energy fuel for nanometer fluorine aluminium height prepared by embodiment two, and 2 be nanometer aluminium powder；
Fig. 3 is the enlarged drawing in the area Tu2Zhong A, and 1 releases energy fuel for nanometer fluorine aluminium height prepared by embodiment two, and 2 be nano aluminum
Powder；
Fig. 4 is TG figure, and 1 releases energy fuel for nanometer fluorine aluminium height prepared by embodiment two, and 2 be nanometer aluminium powder；
Fig. 5 is infrared thermal imaging figure when nanometer fluorine aluminium height prepared by embodiment two releases energy ignited fuel 0s；
Fig. 6 is infrared thermal imaging figure when nanometer fluorine aluminium height prepared by embodiment two releases energy ignited fuel 0.8s；
Fig. 7 is infrared thermal imaging figure when nanometer fluorine aluminium height prepared by embodiment two releases energy ignited fuel 1.44s；
Fig. 8 is infrared thermal imaging figure when nanometer fluorine aluminium height prepared by embodiment two releases energy ignited fuel 1.8s；
Fig. 9 is infrared thermal imaging figure when nanometer fluorine aluminium height prepared by embodiment two releases energy ignited fuel 2.4s；
Figure 10 is infrared thermal imaging figure when nanometer fluorine aluminium height prepared by embodiment two releases energy ignited fuel 3s；
Figure 11 is infrared thermal imaging figure when nanometer aluminium powder lights 0s；
Figure 12 is infrared thermal imaging figure when nanometer aluminium powder lights 0.4s；
Figure 13 is infrared thermal imaging figure when nanometer aluminium powder lights 0.52s；
Figure 14 is infrared thermal imaging figure when nanometer aluminium powder lights 0.92s；
Figure 15 is infrared thermal imaging figure when nanometer aluminium powder lights 1.32s；
Figure 16 is infrared thermal imaging figure when nanometer aluminium powder lights 1.72s；
Figure 17 is the XRD diagram that nanometer fluorine aluminium height prepared by embodiment two releases energy fuel.
Specific embodiment
Specific embodiment 1: the nanometer fluorine aluminium height of present embodiment release can fuel by go oxide film dissolving nanometer aluminium core and
Shell composition；HF solution processing nanometer aluminium core obtains the nanometer aluminium core of oxide film dissolving, while generating Al2F1.5(OH)1.5·
0.375H2O silicon source, then with Al2F1.5(OH)1.5·0.375H2It is aluminium cross-linked that O silicon source and perfluorocarboxylic acid react the perfluorocarboxylic acid to be formed
Network is as shell.
The beneficial effect of present embodiment is: 1, present embodiment is that a kind of aluminium cross-linked network of perfluorocarboxylic acid is built
Vertical class high polymer clad directly contacts to form nanometer fluorine aluminum compound structure with active aluminium core, and specific the reaction mechanism is as follows: (1) HF
The oxide layer on solution etches aluminium powder surface, simultaneous reactions generate intermediate A l2F1.5(OH)1.5·0.375H2O；(2) intermediate
Al2F1.5(OH)1.5·0.375H2O is formed by micelle with perfluorocarboxylic acid and carries out reacting generation perfluoro caprylic acid aluminium group；(3) complete simultaneously
Fluorine aluminium octoate forms final composite construction due to the spontaneous generation crosslinking of the characteristic of its hydrophobic oleophobic.This method removes nanometer aluminium powder
While surface film oxide, construct one layer of fluorine-containing shell similar with its thickness, surface coating layer thickness in 5nm or so, with
Former oxidation film is compared to almost the same.Wherein, the perfluorocarboxylic acid coating of 5nm or so, and this can be constructed when perfluorocarboxylic acid is appropriate
When coating can be clearly seen as single layer, micelle is in the evenly distributed generation in aluminium core surface.Clad is blocked up, and will lead to aluminium powder surface has
Organic coating is excessive, and active aluminium content decline reduces its total enthalpy.
2, the nanometer fluorine aluminium height of present embodiment preparation is released energy fuel and is shown on maximum DSC in the first heat release step
Heat release is 154W/g, and corresponding to pure aluminium powder in the first heat release step heat release maximum value is 15.5W/g, occurs nearly ten times and mentions
It rises.Perfluorocarboxylic acid clad plays extremely critical effect herein, and organic coating decomposes (150 DEG C -400 DEG C) at low temperature
So that there is one layer of very thin AlF in aluminium powder surface3Shell.After being gradually warmed up, the shell moment is broken, completes inside entire aluminium powder
Oxidation, while releasing big calorimetric.
3, the nanometer fluorine aluminium height of present embodiment preparation releases energy fuel, and reaction condition is mild, is suitable for fairly large
Production.
Specific embodiment 2: the preparation method that a kind of nanometer of fluorine aluminium height of present embodiment releases energy fuel is by following step
It is rapid to carry out:
One, the HF solution that mass percent is 1%~10% is mixed with solvent, obtains mixed solution；
The volume ratio of HF solution and solvent that the mass percent is 1%~10% is 1:(0.5~2)；
Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature 3min~10min obtains the mixed solution containing aluminium powder；
Nanometer described in the volume and step 2 of the HF solution that mass percent described in step 1 is 1%~10%
The mass ratio of aluminium powder is 10mL:(1~3) g；
Three, the perfluorocarboxylic acid solution that concentration is 5g/L~20g/L, stirring at normal temperature 2h are added into the mixed solution containing aluminium powder
~8h, obtains crude product；
The concentration is that solvent is identical as solvent described in step 1 in the perfluorocarboxylic acid solution of 5g/L~20g/L；
Concentration described in the quality and step 3 of nanometer aluminium powder described in step 2 is the perfluor carboxylic of 5g/L~20g/L
The volume ratio of acid solution is 1g:(10~20) mL；
Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.
Specific embodiment 3: present embodiment is unlike specific embodiment two: solvent described in step 1
For N,N-dimethylformamide, dimethyl acetamide or dimethyl sulfoxide.It is other to be identical with embodiment two.
Specific embodiment 4: unlike one of present embodiment and specific embodiment two or three: institute in step 3
The perfluorocarboxylic acid solution that the concentration stated is 5g/L~20g/L be concentration be 5g/L~20g/L perfluoro decanoate solution, concentration be
The perfluoro caprylic acid solution or concentration of 5g/L~20g/L is the perfluorobutyric acid solution of 5g/L~20g/L.Other and specific embodiment
Two or three is identical.
Specific embodiment 5: unlike one of present embodiment and specific embodiment two to four: will in step 1
The HF solution that mass percent is 1%~5% is mixed with solvent, obtains mixed solution.Other and specific embodiment two to four
It is identical.
Specific embodiment 6: unlike one of present embodiment and specific embodiment two to five: in step 2 to
Nanometer aluminium powder is added in mixed solution, stirring at normal temperature 3min~5min obtains the mixed solution containing aluminium powder.Other and specific implementation
Mode two to five is identical.
Specific embodiment 7: unlike one of present embodiment and specific embodiment two to six: in step 3 to
The perfluorocarboxylic acid solution that concentration is 5g/L~15g/L is added in mixed solution containing aluminium powder, stirring at normal temperature 2h~4h is slightly produced
Object.It is other identical as specific embodiment two to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment two to seven: will in step 1
The HF solution that mass percent is 1%~2.5% is mixed with solvent, obtains mixed solution.It is other with specific embodiment two to
Seven is identical.
Specific embodiment 9: unlike one of present embodiment and specific embodiment two to eight: in step 3 to
The perfluorocarboxylic acid solution that concentration is 5g/L~10g/L is added in mixed solution containing aluminium powder, stirring at normal temperature 2h~5h is slightly produced
Object.It is other identical as specific embodiment two to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment two to nine: will in step 1
The HF solution that mass percent is 1%~3% is mixed with solvent, obtains mixed solution.Other and specific embodiment two to nine
It is identical.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
Nanometer fluorine aluminium height is released energy fuel and is made of the nanometer aluminium core and shell for removing oxide film dissolving；HF solution handles nanometer aluminium core
The nanometer aluminium core of oxide film dissolving is obtained, while generating Al2F1.5(OH)1.5·0.375H2O silicon source, then with Al2F1.5(OH)1.5·
0.375H2O silicon source and perfluorocarboxylic acid react the aluminium cross-linked network of the perfluorocarboxylic acid to be formed as shell；
The preparation method that above-mentioned nanometer fluorine aluminium height releases energy fuel is to sequentially include the following steps:
One, the HF solution that mass percent is 5% is mixed with solvent, obtains mixed solution；
The solvent is N,N-dimethylformamide；
The volume ratio of HF solution and solvent that the mass percent is 5% is 1:2；
Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature 5min obtains the mixed solution containing aluminium powder；
Nanometer aluminium powder described in the volume and step 2 of the HF solution that mass percent described in step 1 is 5%
Mass ratio is 10mL:2g；
Three, the N,N-dimethylformamide that the perfluoro decanoate that concentration is 15g/L is added into the mixed solution containing aluminium powder is molten
Liquid, stirring at normal temperature 4h, obtains crude product；
Concentration described in the quality and step 3 of nanometer aluminium powder described in step 2 is the N of the perfluoro decanoate of 15g/L,
The volume ratio of dinethylformamide solution is 1g:20mL；
Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.
Embodiment two:
Nanometer fluorine aluminium height is released energy fuel and is made of the nanometer aluminium core and shell for removing oxide film dissolving；HF solution handles nanometer aluminium core
The nanometer aluminium core of oxide film dissolving is obtained, while generating Al2F1.5(OH)1.5·0.375H2O silicon source, then with Al2F1.5(OH)1.5·
0.375H2O silicon source and perfluorocarboxylic acid react the aluminium cross-linked network of the perfluorocarboxylic acid to be formed as shell；
The preparation method that above-mentioned nanometer fluorine aluminium height releases energy fuel is to sequentially include the following steps:
One, the HF solution that mass percent is 2.5% is mixed with solvent, obtains mixed solution；
The solvent is dimethyl sulfoxide；
The volume ratio of HF solution and solvent that the mass percent is 2.5% is 1:1.3；
Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature 5min obtains the mixed solution containing aluminium powder；
Nanometer aluminium powder described in the volume and step 2 of the HF solution that mass percent described in step 1 is 2.5%
Mass ratio be 10mL:1.3g；
Three, the dimethyl sulphoxide solution for the perfluoro caprylic acid that concentration is 10g/L, room temperature are added into the mixed solution containing aluminium powder
2h is stirred, crude product is obtained；
Concentration described in the quality and step 3 of nanometer aluminium powder described in step 2 is the two of the perfluoro caprylic acid of 10g/L
The volume ratio of methyl sulfoxide solution is 1g:10mL；
Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.
Fig. 1 is the TEM figure that nanometer fluorine aluminium height prepared by embodiment two releases energy fuel；As seen from the figure, nanometer fluorine aluminium height releases energy
Coating thickness is 5nm or so in fuel.
Fig. 2 is DSC figure, and 1 releases energy fuel for nanometer fluorine aluminium height prepared by embodiment two, and 2 be nanometer aluminium powder；Fig. 3 is in Fig. 2
The enlarged drawing in the area A, 1 releases energy fuel for nanometer fluorine aluminium height prepared by embodiment two, and 2 be nanometer aluminium powder；As seen from the figure, nanometer is compared
Aluminium powder, nanometer fluorine aluminium height manufactured in the present embodiment release energy fuel, show that heat release is in the first heat release step, on maximum DSC
154W/g, and corresponding to nanometer aluminium powder in the first heat release step heat release maximum value is 15.5W/g, nearly ten times of promotion occurs, together
When in enlarged drawing it is found that when its decomposition, generates gas and nanometer aluminium powder exothermic heat of reaction.
Fig. 4 is TG figure, and 1 releases energy fuel for nanometer fluorine aluminium height prepared by embodiment two, and 2 be nanometer aluminium powder；As seen from the figure, originally
The nanometer fluorine aluminium height of embodiment preparation releases energy fuel, and first weightlessness increases weight again, and fluorine-containing object divides in the corresponding fluorine aluminium composite material of weightlessness
Solution.
Fig. 5 is infrared thermal imaging figure when nanometer fluorine aluminium height prepared by embodiment two releases energy ignited fuel 0s；Fig. 6 is to implement
Nanometer fluorine aluminium height prepared by example two releases infrared thermal imaging figure when energy ignited fuel 0.8s；Fig. 7 is nanometer prepared by embodiment two
Fluorine aluminium height releases infrared thermal imaging figure when energy ignited fuel 1.44s；Fig. 8 is that nanometer fluorine aluminium height prepared by embodiment two releases energy fuel
Light infrared thermal imaging figure when 1.8s；Fig. 9 be embodiment two prepare nanometer fluorine aluminium height release can ignited fuel 2.4s when it is red
Outer thermograph；Figure 10 is infrared thermal imaging figure when nanometer fluorine aluminium height prepared by embodiment two releases energy ignited fuel 3s；
Figure 11 is infrared thermal imaging figure when nanometer aluminium powder lights 0s；Figure 12 is infrared heat when nanometer aluminium powder lights 0.4s
Image；Figure 13 is infrared thermal imaging figure when nanometer aluminium powder lights 0.52s；Figure 14 is red when nanometer aluminium powder lights 0.92s
Outer thermograph；Figure 15 is infrared thermal imaging figure when nanometer aluminium powder lights 1.32s；When Figure 16 is that nanometer aluminium powder lights 1.72s
Infrared thermal imaging figure；In summary, comparison nanometer aluminium powder and nanometer fluorine aluminium height release the misfire of energy fuel, find nanometer fluorine
The firing temperature that aluminium height releases energy fuel reduces, this is because the generation of PIR process, nanometer fluorine aluminium height is released in entire combustion process
The highest flame temperature of energy fuel has reached 1367 DEG C of flame temperatures for being significantly larger than nanometer aluminium powder, and this phenomenon and this reality
It applies corresponding to the thermogravimetric test of example.
Figure 17 is the XRD diagram that nanometer fluorine aluminium height prepared by embodiment two releases energy fuel；It can be seen that nanometer aluminium powder itself
It does not change, while occurring at 15.7 °, 30.3 °, 31.7 °, 36.8 °, 48.4 ° and 53.0 ° (ICSD No.74-0940)
Some impurity peaks show that it etches nanometer aluminium core (aluminium oxide) for HF through analysis, obtained by-product Al2F1.5(OH)1.5·
0.375H2O silicon source.
Embodiment three:
Nanometer fluorine aluminium height is released energy fuel and is made of the nanometer aluminium core and shell for removing oxide film dissolving；HF solution handles nanometer aluminium core
The nanometer aluminium core of oxide film dissolving is obtained, while generating Al2F1.5(OH)1.5·0.375H2O silicon source, then with Al2F1.5(OH)1.5·
0.375H2O silicon source and perfluorocarboxylic acid react the aluminium cross-linked network of the perfluorocarboxylic acid to be formed as shell；
The preparation method that above-mentioned nanometer fluorine aluminium height releases energy fuel is to sequentially include the following steps:
One, the HF solution that mass percent is 3% is mixed with solvent, obtains mixed solution；
The solvent is dimethyl acetamide；
The volume ratio of HF solution and solvent that the mass percent is 3% is 1:1.3；
Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature 5min obtains the mixed solution containing aluminium powder；
Nanometer aluminium powder described in the volume and step 2 of the HF solution that mass percent described in step 1 is 3%
Mass ratio is 10mL:1g；
Three, the dimethylacetamide solution for the perfluorobutyric acid that concentration is 7g/L is added into the mixed solution containing aluminium powder, often
Temperature stirring 2h, obtains crude product；
Concentration described in the quality and step 3 of nanometer aluminium powder described in step 2 is the two of the perfluorobutyric acid of 7g/L
The volume ratio of methyl vinyl amine aqueous solution is 1g:12mL；
Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.
Example IV:
Nanometer fluorine aluminium height is released energy fuel and is made of the nanometer aluminium core and shell for removing oxide film dissolving；HF solution handles nanometer aluminium core
The nanometer aluminium core of oxide film dissolving is obtained, while generating Al2F1.5(OH)1.5·0.375H2O silicon source, then with Al2F1.5(OH)1.5·
0.375H2O silicon source and perfluorocarboxylic acid react the aluminium cross-linked network of the perfluorocarboxylic acid to be formed as shell；
The preparation method that above-mentioned nanometer fluorine aluminium height releases energy fuel is to sequentially include the following steps:
One, the HF solution that mass percent is 6% is mixed with solvent, obtains mixed solution；
The solvent is dimethyl acetamide；
The volume ratio of HF solution and solvent that the mass percent is 6% is 1:1；
Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature 5min obtains the mixed solution containing aluminium powder；
Nanometer aluminium powder described in the volume and step 2 of the HF solution that mass percent described in step 1 is 6%
Mass ratio is 10mL:3g；
Three, the dimethylacetamide solution for the perfluorobutyric acid that concentration is 5g/L is added into the mixed solution containing aluminium powder, often
Temperature stirring 2h, obtains crude product；
Concentration described in the quality and step 3 of nanometer aluminium powder described in step 2 is the two of the perfluorobutyric acid of 5g/L
The volume ratio of methyl vinyl amine aqueous solution is 1g:20mL；
Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.
Embodiment five:
Nanometer fluorine aluminium height is released energy fuel and is made of the nanometer aluminium core and shell for removing oxide film dissolving；HF solution handles nanometer aluminium core
The nanometer aluminium core of oxide film dissolving is obtained, while generating Al2F1.5(OH)1.5·0.375H2O silicon source, then with Al2F1.5(OH)1.5·
0.375H2O silicon source and perfluorocarboxylic acid react the aluminium cross-linked network of the perfluorocarboxylic acid to be formed as shell；
The preparation method that above-mentioned nanometer fluorine aluminium height releases energy fuel is to sequentially include the following steps:
One, the HF solution that mass percent is 5% is mixed with solvent, obtains mixed solution；
The solvent is N,N-dimethylformamide；
The volume ratio of HF solution and solvent that the mass percent is 5% is 1:1.3；
Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature 5min obtains the mixed solution containing aluminium powder；
The mass ratio of nanometer aluminium powder described in the HF solution and step 2 that mass percent described in step 1 is 5%
For 10mL:2.5g；
Three, the n,N-Dimethylformamide solution for the perfluoro caprylic acid that concentration is 6/L is added into the mixed solution containing aluminium powder,
Stirring at normal temperature 2h, obtains crude product；
Concentration described in the quality and step 3 of nanometer aluminium powder described in step 2 is the N of the perfluoro caprylic acid of 6g/L,
The volume ratio of dinethylformamide solution is 1g:18mL；
Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.
Claims (10)
1. a kind of nanometer of fluorine aluminium height is released can fuel, it is characterised in that nanometer fluorine aluminium height release can fuel by going the nano aluminum of oxide film dissolving
Core and shell composition；HF solution processing nanometer aluminium core obtains the nanometer aluminium core of oxide film dissolving, while generating Al2F1.5
(OH)1.5·0.375H2O silicon source, then with Al2F1.5(OH)1.5·0.375H2O silicon source and perfluorocarboxylic acid react the perfluor carboxylic to be formed
The aluminium cross-linked network of acid is as shell.
2. the preparation method that a kind of nanometer of fluorine aluminium height as described in claim 1 releases energy fuel, it is characterised in that a kind of nanometer of fluorine
The preparation method that aluminium height releases energy fuel is to sequentially include the following steps:
One, the HF solution that mass percent is 1%~10% is mixed with solvent, obtains mixed solution；
The volume ratio of HF solution and solvent that the mass percent is 1%~10% is 1:(0.5~2)；
Two, nanometer aluminium powder is added into mixed solution, stirring at normal temperature 3min~10min obtains the mixed solution containing aluminium powder；
Nanometer aluminium powder described in the volume and step 2 of the HF solution that mass percent described in step 1 is 1%~10%
Mass ratio be 10mL:(1~3) g；
Three, the perfluorocarboxylic acid solution that addition concentration is 5g/L~20g/L into the mixed solution containing aluminium powder, stirring at normal temperature 2h~
8h obtains crude product；
The concentration is that solvent is identical as solvent described in step 1 in the perfluorocarboxylic acid solution of 5g/L~20g/L；
Concentration described in the quality and step 3 of nanometer aluminium powder described in step 2 is that the perfluorocarboxylic acid of 5g/L~20g/L is molten
The volume ratio of liquid is 1g:(10~20) mL；
Four, crude product is washed and is filtered under diminished pressure using dehydrated alcohol, obtained a nanometer fluorine aluminium height and release energy fuel.
3. the preparation method that a kind of nanometer of fluorine aluminium height according to claim 2 releases energy fuel, it is characterised in that in step 1
The solvent is N,N-dimethylformamide, dimethyl acetamide or dimethyl sulfoxide.
4. the preparation method that a kind of nanometer of fluorine aluminium height according to claim 2 releases energy fuel, it is characterised in that in step 3
The perfluorocarboxylic acid solution that the concentration is 5g/L~20g/L be concentration be 5g/L~20g/L perfluoro decanoate solution, concentration be
The perfluoro caprylic acid solution or concentration of 5g/L~20g/L is the perfluorobutyric acid solution of 5g/L~20g/L.
5. the preparation method that a kind of nanometer of fluorine aluminium height according to claim 2 releases energy fuel, it is characterised in that in step 1
The HF solution that mass percent is 1%~5% is mixed with solvent, obtains mixed solution.
6. the preparation method that a kind of nanometer of fluorine aluminium height according to claim 2 releases energy fuel, it is characterised in that in step 2
Nanometer aluminium powder is added into mixed solution, stirring at normal temperature 3min~5min obtains the mixed solution containing aluminium powder.
7. the preparation method that a kind of nanometer of fluorine aluminium height according to claim 2 releases energy fuel, it is characterised in that in step 3
The perfluorocarboxylic acid solution that concentration is 5g/L~15g/L is added into the mixed solution containing aluminium powder, stirring at normal temperature 2h~4h is obtained thick
Product.
8. the preparation method that a kind of nanometer of fluorine aluminium height according to claim 2 releases energy fuel, it is characterised in that in step 1
The HF solution that mass percent is 1%~2.5% is mixed with solvent, obtains mixed solution.
9. the preparation method that a kind of nanometer of fluorine aluminium height according to claim 2 releases energy fuel, it is characterised in that in step 3
The perfluorocarboxylic acid solution that concentration is 5g/L~10g/L is added into the mixed solution containing aluminium powder, stirring at normal temperature 2h~5h is obtained thick
Product.
10. the preparation method that a kind of nanometer of fluorine aluminium height according to claim 2 releases energy fuel, it is characterised in that in step 1
The HF solution that mass percent is 1%~3% is mixed with solvent, obtains mixed solution.
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| CN110508802A (en) * | 2019-08-29 | 2019-11-29 | 南京理工大学 | The preparation method of polyvinylidene fluoride cladding micro-/ nano aluminium powder |
| CN111574314A (en) * | 2020-05-21 | 2020-08-25 | 中国科学院兰州化学物理研究所 | Method for improving stability and combustion performance by modifying aluminum powder with fluoroalkyl compound |
| CN113501740A (en) * | 2021-07-08 | 2021-10-15 | 中国工程物理研究院化工材料研究所 | Preparation method of surface fluorination modified nano aluminum powder |
| CN115703690A (en) * | 2021-08-09 | 2023-02-17 | 北京理工大学 | Perfluoro-copper octoate-aluminum powder energetic composite particle and preparation method thereof |
| CN115703690B (en) * | 2021-08-09 | 2024-04-26 | 北京理工大学 | Copper perfluorooctanoate-aluminum powder energetic composite particles and preparation method thereof |
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| CN110508802A (en) * | 2019-08-29 | 2019-11-29 | 南京理工大学 | The preparation method of polyvinylidene fluoride cladding micro-/ nano aluminium powder |
| WO2021036679A1 (en) * | 2019-08-29 | 2021-03-04 | 南京理工大学 | Method for preparing polyvinylidene fluoride-coated micro-nano aluminum powder |
| CN111574314A (en) * | 2020-05-21 | 2020-08-25 | 中国科学院兰州化学物理研究所 | Method for improving stability and combustion performance by modifying aluminum powder with fluoroalkyl compound |
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| CN115703690A (en) * | 2021-08-09 | 2023-02-17 | 北京理工大学 | Perfluoro-copper octoate-aluminum powder energetic composite particle and preparation method thereof |
| CN115703690B (en) * | 2021-08-09 | 2024-04-26 | 北京理工大学 | Copper perfluorooctanoate-aluminum powder energetic composite particles and preparation method thereof |
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