CN115282994B - Preparation method and application of high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride - Google Patents
Preparation method and application of high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride Download PDFInfo
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Abstract
The invention relates to a preparation method and application of a high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride, wherein a dispersing agent is added into a graphite carbon nitride suspension to obtain a mixed solution A, and a nano aluminum powder suspension and a nano copper ferrite suspension are uniformly mixed to obtain a mixed solution B; and mixing the mixed solution A and the mixed solution B, performing ultrasonic treatment to form sol, and performing vacuum freeze drying on the sol to obtain the high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride. The high-energy composite material prepared by the invention has ultrahigh dispersibility and ultralow density; meanwhile, the metal composite oxide and the metal fuel can generate sustainable severe oxidation-reduction reaction and release huge energy; can be used as a combustion catalyst of the solid propellant, realizes the rapid steady-state combustion of the solid propellant, and reduces the pressure index. The synthesis method is green, safe, simple and effective, has good environment and is easy for industrial production.
Description
Technical Field
The invention belongs to the technical field of nano energetic materials, and particularly relates to a preparation method and application of a high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride.
Background
High reactive metastable mixed complexes (MICs) have attracted considerable attention due to their higher energy density and good combustion performance. Nano thermite is one of MICs and is a heterogeneous mixture composed of metal fuels (aluminum, boron, magnesium, etc.) with nano-scale and inorganic oxidants (metal oxides). Wherein at least one component of the nanocomposite should be nanoscale, which properties make these materials different from microscale Energetic Materials (EMs). In order to further improve the properties of MICs, various novel components (e.g., carbon nanomaterial), structures (biomimetic interface), and preparation methods (sol-gel and electrospinning) have been developed in recent years. The new compositions and structures have been found to be effective in improving ignition and combustion characteristics, while advanced manufacturing processes can optimize the safety and cost of the corresponding MICs. By all these means, MICs are obtained that are safe, green, inexpensive and have tunable properties.
Nano metal composite oxide due to multiple groupsThe metal oxide is doped mutually, and the charge transfer between different components causes lattice distortion, so that more active sites are formed in a crystal structure, and the metal oxide has more excellent performance than a single component metal oxide. In addition, graphite carbon nitride (g-C 3 N 4 ) Is a novel typical polymer semiconductor, has a planar two-dimensional lamellar structure similar to graphene, and is bonded between nano-sheets by Van der Waals force. Compared with GO, g-C 3 N 4 The preparation process flow is short and simple, and the cost is low. And g-C 3 N 4 The catalyst has the advantages of wide absorption spectrum range, high catalytic activity, good thermal stability and chemical stability, no toxicity and pollution, no noble metal and larger specific surface area, and can effectively reduce agglomeration of nano particles, increase interfacial contact between components and improve ignition and combustion performance.
Unlike traditional self-assembly process of preparing metal composite oxide/GO/Al, the self-assembly may be realized successfully through long-range electrostatic interaction and recombination of Van der Waals force and positively charged nanometer particle. And g-C 3 N 4 The electronegativity is weak, layering occurs after the mixture of the metal composite oxide and nano Al and centrifugation, and self-assembly cannot be realized.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a preparation method and application of a high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride, and the composite material has good dispersibility and small density and can be used for thermal decomposition of energetic materials.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a high energy composite material based on copper ferrite, aluminum and graphite carbon nitride, comprising the steps of:
adding a dispersing agent into the graphite carbon nitride suspension to obtain a mixed solution A, and uniformly mixing the nano aluminum powder suspension and the nano copper ferrite suspension to obtain a mixed solution B;
and mixing the mixed solution A and the mixed solution B, performing ultrasonic treatment to form sol, and performing vacuum freeze drying on the sol to obtain the high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride.
Further, the graphite carbon nitride suspension is prepared by the following process: adding graphite carbon nitride into a solvent for ultrasonic treatment to prepare graphite carbon nitride suspension;
the Al powder suspension is prepared by the following steps: adding nano aluminum powder into a solvent for ultrasonic treatment to prepare nano aluminum powder suspension;
the nano copper ferrite suspension is prepared by the following steps: adding nano copper ferrite into a solvent, and performing ultrasonic treatment to obtain nano copper ferrite suspension.
Further, the particle size of the nano aluminum powder is 80-300nm.
Further, the particle size of the nano copper ferrite is 150-300nm.
Further, the solvent is tertiary butanol, and the dispersing agent is PVP.
Further, the total mass of graphite carbon nitride, nano aluminum powder and nano copper ferrite corresponding to each 1mL of tertiary butanol is 5-10mg.
Further, the dispersant is used in an amount of 3 to 5wt% based on the high energy composite of copper ferrite, aluminum and graphite carbon nitride.
Further, the amount of graphite carbon nitride is 1 to 7.5wt% based on the weight of the high energy composite material of copper ferrite, aluminum and graphite carbon nitride; the ratio of the amount of the nano aluminum powder to the nano copper ferrite is 2.0:1-4.7:1.
A high energy composite material based on copper ferrite, aluminum and graphite carbon nitride prepared according to the method described above is applied as a nano thermite.
Use of a high energy composite material based on copper ferrite, aluminium and graphite carbon nitride prepared according to the method described above as a catalyst for thermal decomposition of energetic materials.
Compared with the prior art, the invention has the following beneficial effects:
the high-energy composite material Al/CuFe prepared by the invention 2 O 4 /g-C 3 N 4 At the same time have metal composite oxide CuFe 2 O 4 And metal fuel Al, can generate sustainable severe oxidation reductionReacting and releasing huge energy; meanwhile, the metal composite oxide CuFe 2 O 4 More oxygen can be provided for the oxidation-reduction reaction of the composite material, so that the energy release is further improved; g-C 3 N 4 The two-dimensional nano sheet structure and a plurality of excellent characteristics are rich in N element, and the preparation process is simple and the price is low. g-C under the action of dispersing agent 3 N 4 Can be well matched with CuFe 2 O 4 And the composite material is compounded with metal fuel Al, so that the interface contact area between two phases is increased, the agglomeration of nano particles can be effectively inhibited, the dispersibility is improved, and the full reaction of the composite material is facilitated. The synthesis method is simple, safe and effective, has good environment and is easy for industrial production; the method is obviously different from the traditional self-assembly method, effectively solves the problem of uneven mixing of the components in the nano thermite, and greatly improves the dispersibility of the prepared material. And the prepared high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 The density is small and the specific volume is large.
The high-energy composite material Al/CuFe synthesized by the invention 2 O 4 /g-C 3 N 4 Combustion catalyst capable of being used as solid propellant and having better catalytic effect on thermal decomposition of energetic materials (such as AP, TKX-50) than single-component Al and g-C 3 N 4 The rapid steady-state combustion of the solid propellant is realized, and the pressure index is reduced.
Drawings
FIG. 1 is an Al/CuFe alloy of example 2 2 O 4 /g-C 3 N 4 A sample photograph; wherein, (a) is a schematic diagram, (b) is a size schematic diagram, and (c) is a weight diagram.
FIG. 2 shows the components of example 2 and the Al/CuFe mixture 2 O 4 /g-C 3 N 4 Standing for 0h and 24h in tertiary butanol in an ultrasonic dispersion way; wherein (a) is Al suspension and CuFe 2 O 4 Suspension with g-C 3 N 4 The mixture of the suspensions was left for 0h, (b) for Al suspension for 0h, (c) for CuFe 2 O 4 The suspension was left for 0h, with (d) g-C 3 N 4 The suspension is placed for 0h, and (e) is Al suspension and CuFe 2 O 4 Suspension with g-C 3 N 4 The mixture of the suspensions was left for 24h, (f) for Al suspension for 24h, (g) for CuFe 2 O 4 The suspension was left for 24h, g-C (h) 3 N 4 The suspension was left for 24h.
FIG. 3 is an Al/CuFe alloy of example 2 2 O 4 /g-C 3 N 4 SEM and TEM images of (a); wherein (a) is g-C 3 N 4 SEM images of (a); (b) Is CuFe 2 O 4 SEM images of (a); (c) Is Al/CuFe 2 O 4 /g-C 3 N 4 (d) is Al/CuFe 2 O 4 /g-C 3 N 4 A TEM image of (a);
FIG. 4 is an Al/CuFe alloy of example 2 2 O 4 /g-C 3 N 4 XRD pattern of (a);
FIG. 5 shows the Al/CuFe of examples 1-3 2 O 4 /g-C 3 N 4 Is a DSC graph of (2);
FIG. 6 is a DSC graph of thermal decomposition of AP and TKX-50 in the presence of different catalysts; wherein, (a) is AP and (b) is TKX-50;
FIG. 7 is a graph comparing the use of PEG and ethylene glycol as dispersants and solvents during the preparation process; wherein, (a) is tertiary butanol as a solvent, PVP is selected as a dispersing agent, (b) is tertiary butanol as a solvent, PEG is selected as a dispersing agent, (c) is a sample photo of the product obtained by freeze drying in the graph (a), (d) is a sample photo of the product obtained by freeze drying in the graph (b), (e) is ethylene glycol as a solvent, PVP is selected as a dispersing agent, (f) is ethylene glycol as a solvent, and PEG is selected as a dispersing agent.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
The following are specific examples to further illustrate the technical scheme of the present invention.
The high-energy composite material Al/CuFe of the invention 2 O 4 /g-C 3 N 4 The preparation method of (2) comprises the following steps: graphite carbon nitride (g-C) was first prepared separately 3 N 4 ) Suspension, nano aluminum powder (Al) suspension, and nano copper ferrite (CuFe) 2 O 4 ) A suspension;
g-C 3 N 4 the suspension is prepared by the following process: will g-C 3 N 4 Adding into solvent, and ultrasonic treating to obtain g-C 3 N 4 A suspension;
the Al powder suspension is prepared by the following steps: adding nano Al into a solvent for ultrasonic treatment to prepare Al powder suspension;
CuFe 2 O 4 the suspension is prepared by the following process: nano CuFe 2 O 4 Adding into solvent, and performing ultrasonic treatment to obtain CuFe 2 O 4 A suspension.
Then adding a certain amount of dispersing agent PVP to g-C 3 N 4 In the suspension, a mixed solution A is obtained, and Al powder suspension and CuFe are mixed according to a certain proportion 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B; mixing the obtained mixed solution A and mixed solution B, continuing to carry out ultrasonic treatment to form sol, and finally carrying out vacuum freeze drying to obtain the Al/CuFe 2 O 4 /g-C 3 N 4 And (5) a product.
The grain diameter of the nano Al is 80-300nm, and the nano CuFe 2 O 4 The particle size of (2) is about 150-300nm.
The solvent used in the preparation of the suspension in the present invention is t-butanol, g-C per 1mL of t-butanol 3 N 4 Nano Al and CuFe 2 O 4 The total mass of the catalyst is 5-10mg, i.e. the solvent dosage is about 5-10 mg.mL -1 。
The PVP in the invention is 3-5wt% of the composite material.
The ultrasonic time is 2-4 hours; g-C 3 N 4 The dosage of (C) is Al/CuFe 2 O 4 /g-C 3 N 4 1 to 7.5wt% of the weight of (C); al and CuFe 2 O 4 The ratio of the amounts of the substances is 2.0:1 to 4.7:1.
Al/CuFe 2 O 4 /g-C 3 N 4 Can be used as a nano thermite.
Al/CuFe 2 O 4 /g-C 3 N 4 Can be used as a thermal decomposition catalyst of energy-containing materials (such as AP and TKX-50).
Example 1
(1) 30.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 Is a suspension of (a); 116.0mg of nano Al powder (purity 99.5%) and 254.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％，g-C 3 N 4 ＝7.5wt％)。
Example 2
(1) 20.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 Is a suspension of (a); 118.0mg of nano Al powder (purity: 99.5%) and 262.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％，g-C 3 N 4 ＝5wt％)。
In FIG. 1 (a), (b)And (c) Al/CuFe prepared in example 2 2 O 4 /g-C 3 N 4 An optical photograph; the results show that: al/CuFe prepared by the method 2 O 4 /g-C 3 N 4 The energetic composite material exhibits the same shape as the host container. By measuring the mass (m= 0.33412 g) and volume (v=9.42 cm 3 ) Data, calculated density of sample is 0.035g cm -3 Specific volume of 28.57cm 3 ·g -1 Indicating that the sample has ultra-light mass and ultra-low density.
In FIG. 2, (a), (b), (c), (d), (e), (f), (g) and (h) are Al and CuFe obtained in example 2 2 O 4 、g-C 3 N 4 Al/CuFe 2 O 4 /g-C 3 N 4 Standing for 0h and 24h in tertiary butanol in an ultrasonic dispersion way; the results show that the components and the mixed Al/CuFe 2 O 4 /g-C 3 N 4 After ultrasonic standing for 24 hours, the mixture is basically unchanged, and no layering or precipitation occurs, which indicates Al/CuFe 2 O 4 /g-C 3 N 4 Has higher dispersivity.
In FIG. 3 (a) is g-C 3 N 4 (b) is CuFe 2 O 4 (c) and (d) are the Al/CuFe obtained in example 2 2 O 4 /g-C 3 N 4 SEM and TEM images of (a) and (b) indicating that: g-C 3 N 4 Exhibiting a uniform nano-platelet structure. Nano CuFe with rough surface 2 O 4 The particles and the nanometer Al particles with smooth surfaces are uniformly mixed and are uniformly loaded on g-C 3 N 4 On the nano-sheet, the interface contact area between the components is increased.
FIG. 4 shows the Al/CuFe composition prepared in example 2 2 O 4 /g-C 3 N 4 The results show that: al/CuFe 2 O 4 /g-C 3 N 4 Diffraction peaks of XRD profile of (C) with CuFe 2 O 4 Standard cards of (JCPDS No. 77-0010) and Al (JCPDS No. 04-0787) were identical, and weak g-C was observed at 2θ=27.5° 3 N 4 Characteristic peaks of (2) indicating Al/CuFe 2 O 4 /g-C 3 N 4 Successful preparation of high energy composite materials.
DSC test after mixing with AP and TKX-50:
the high energy composite Al/CuFe obtained in example 2 2 O 4 /g-C 3 N 4 The content of the TKX-50 and the AP are respectively 1:4, uniformly mixing at a heating rate of 10 ℃ for min -1 DSC measurement was performed under the conditions, and the results shown in (a) and (b) in FIG. 6 were obtained. The melting peak temperature of the pure AP does not change obviously, the two exothermic decomposition peak temperatures of the AP are 309.2 and 240.3 ℃ respectively, and Al/CuFe 2 O 4 /g-C 3 N 4 The addition of (3) causes the two exothermic decomposition peaks of the AP to be combined into one, the peak temperature is reduced by 70.4 ℃, and the apparent activation energy is reduced by 119.5 kJ.mol compared with that of pure AP -1 The method comprises the steps of carrying out a first treatment on the surface of the Pure TKX-50 has a decomposition peak temperature of 240.9 ℃ and Al/CuFe 2 O 4 /g-C 3 N 4 The main peak temperature of TKX-50 is reduced by 34.3 ℃, and the catalyst has remarkable catalytic decomposition effect.
Example 3
(1) 10.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 Is a suspension of (a); 122.0mg of nano Al powder (purity 99.5%) and 268.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 Obtaining a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％，g-C 3 N 4 ＝2.5wt％)。
DSC test:
taking the heights synthesized by the methods of examples 1-3Al/CuFe capable of being compounded 2 O 4 /g-C 3 N 4 (g-C 3 N 4 =2.5, 5.0 and 7.5wt%, at a temperature rise rate of 10 ℃ for min -1 DSC measurement is carried out under the condition to obtain the result shown in figure 5, the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 All decompose at about 580 ℃ and only has one exothermic decomposition peak, indicating that the Al/CuFe 2 O 4 /g-C 3 N 4 The nano thermite has been completely decomposed before the aluminum melts (melting peak of aluminum is about 658 ℃). The exotherm is 653.4, 954.9 and 863.1J g respectively -1 And when g-C 3 N 4 The heat release amount was maximized at =2.5wt%.
Example 4
(1) Will 4.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 Is a suspension of (a); 124.0mg of nano Al powder (purity 99.5%) and 272.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％，g-C 3 N 4 ＝1.0wt％)。
Example 5
(1) 20.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 (5 wt%); 118.0mg of nano Al powder (purity: 99.5%) and 262.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nanoCuFe 2 O 4 A suspension;
(2) 12mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝3wt％)。
Example 6
(1) 20.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 (5 wt%); 118.0mg of nano Al powder (purity: 99.5%) and 262.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 16mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝4wt％)。
Example 7
(1) 20.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 (5 wt%); 70.0mg of nano Al powder (purity 99.5%) and 310.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％，Al:CuFe 2 O 4 ＝2.0:1)。
Example 8
(1) 20.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 (5 wt%); 88.0mg of nano Al powder (purity 99.5%) and 292.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％，Al:CuFe 2 O 4 ＝2.7:1)。
Example 9
(1) 20.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 (5 wt%); 104.0mg of nano Al powder (purity 99.5%) and 276.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％，Al:CuFe 2 O 4 ＝3.3:1)。
Example 10
(1) 20.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 (5 wt%); 131.0mg of nano Al powder (purity 99.5%) and 249.0mg of CuFe are weighed out 2 O 4 Respectively dispersing in 10mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％，Al:CuFe 2 O 4 ＝4.7:1)。
Example 11
(1) 20.0mg g-C 3 N 4 Dispersing in 30mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 Is a suspension of (a); 118.0mg of nano Al powder (purity: 99.5%) and 262.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 25mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 Is mixed with the suspension of (2)Combining the liquid A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％)。
Example 12
(1) 20.0mg g-C 3 N 4 Dispersing in 20mL tertiary butanol solution, and performing ultrasonic treatment for 3h to obtain g-C 3 N 4 Is a suspension of (a); 118.0mg of nano Al powder (purity: 99.5%) and 262.0mg of CuFe were weighed out 2 O 4 Respectively dispersing in 15mL tertiary butanol solution for ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe 2 O 4 A suspension;
(2) 20mg PVP was added to g-C 3 N 4 To obtain a mixed solution A; then suspending Al powder and CuFe 2 O 4 Uniformly mixing the suspension by ultrasonic to obtain a mixed solution B;
(3) Mixing the mixed solution A and the mixed solution B prepared in the step (2) and continuing ultrasonic treatment for 2 hours to form sol;
(4) Vacuum freeze drying the sol to obtain the high-energy composite material Al/CuFe 2 O 4 /g-C 3 N 4 (PVP＝5wt％)。
Al/CuFe prepared by adopting the method 2 O 4 /g-C 3 N 4 The nano-thermite can be used as a combustion catalyst of a solid propellant.
To solve g-C 3 N 4 The invention adopts a sol freeze drying technology to obtain uniformly dispersed Al/CuFe 2 O 4 /g-C 3 N 4 High energy composite materials.
The sol-freeze drying technology of the invention is a novel method for preparing nano energetic composite material, and is characterized in that PVP is selected as the materialDispersing agent, tertiary butanol as solvent. And the dispersing agent can only use PVP, and the solvent can only use tertiary butanol; the reason is that PVP is the most characteristic and excellent performance of N-vinyl amide polymer as a nonionic polymer compound, has an average molecular weight of up to 8000-700000, and is extremely easy to dissolve in water and alcohol organic solvents. In the preparation of the thermite, water cannot be used as a solvent, and small-molecule alcohol cannot be used, so that freeze drying cannot be realized. The selection of the dispersant and the solvent requires that the components be mixed, no delamination occurs, and the dispersant and the solvent can be prepared by vacuum freeze drying. If layering is carried out, the sample is unevenly dispersed, and Al/CuFe cannot be successfully prepared 2 O 4 /g-C 3 N 4 High energy composites affect the final properties. Therefore, the solvent is finally determined to be tert-butanol after comparing with other solvents and dispersing agents, and PVP is adopted as the dispersing agent. Fig. 7 shows a comparative graph of the preparation process using PEG and ethylene glycol as the dispersing agent and the solvent, wherein the solvent used in the graphs (a) and (b) is t-butanol, the dispersing agent is PVP and PEG, the graphs (c) and (d) are photographs of the freeze-dried products in the graphs (a) and (b), the solvents (e) and (f) are ethylene glycol, and the dispersing agent is PVP and PEG. The results show that the PEG is used as a dispersing agent, the sample has obvious layering phenomenon, and the high-dispersivity and ultra-light Al/CuFe can not be obtained after the vacuum freeze drying 2 O 4 /g-C 3 N 4 High energy composite materials. And ethylene glycol is used as a solvent, and the ethylene glycol cannot be successfully freeze-dried due to the low freezing point of the ethylene glycol. Therefore, in the sol freeze drying technology, only PVP can be used as a dispersing agent, and tertiary butanol can be used as a solvent.
The invention adopts a novel sol-freeze drying technology to prepare Al/CuFe 2 O 4 /g-C 3 N 4 The high-energy composite material adopts tertiary butanol as a solvent, PVP as a dispersion medium, and the high-dispersivity and ultra-light Al/CuFe is obtained by vacuum freeze drying technology after adding all components for ultrasonic mixing uniformly 2 O 4 /g-C 3 N 4 High energy composite material having a metal composite oxide (CuFe 2 O 4 ) And a metal fuel (Al), and g-C 3 N 4 Is added to allow the two phases to be mixed homogeneously while g-C 3 N 4 The excellent conductivity and the large specific surface area further enhance the catalytic combustion effect of the solid propellant. The method is green, safe and simple to operate, and is a novel method for efficiently preparing the high-dispersity nano energetic composite material.
Claims (7)
1. The preparation method of the high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride is characterized by comprising the following steps of:
adding a dispersing agent into the graphite carbon nitride suspension to obtain a mixed solution A, and uniformly mixing the nano aluminum powder suspension and the nano copper ferrite suspension to obtain a mixed solution B;
mixing the mixed solution A and the mixed solution B, performing ultrasonic treatment to form sol, and performing vacuum freeze drying on the sol to obtain a high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride;
the graphite carbon nitride suspension is prepared by the following process: adding graphite carbon nitride into a solvent for ultrasonic treatment to prepare graphite carbon nitride suspension;
the Al powder suspension is prepared by the following steps: adding nano aluminum powder into a solvent for ultrasonic treatment to prepare nano aluminum powder suspension;
the nano copper ferrite suspension is prepared by the following steps: adding nano copper ferrite into a solvent for ultrasonic treatment to prepare nano copper ferrite suspension;
the solvent is tertiary butanol and the dispersing agent is PVP.
2. The method for preparing the high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride according to claim 1, wherein the particle size of the nano aluminum powder is 80-300nm.
3. The method for preparing the high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride according to claim 1, wherein the particle size of the nano copper ferrite is 150-300nm.
4. The method for preparing the high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride according to claim 1, wherein the amount of the dispersing agent is 3-5wt% of the high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride.
5. The method for preparing the high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride according to claim 1, wherein the dosage of the graphite carbon nitride is 1-7.5wt% based on the weight of the high-energy composite material of copper ferrite, aluminum and graphite carbon nitride; the ratio of the amount of the nano aluminum powder to the nano copper ferrite is 2.0:1-4.7:1.
6. Use of a high energy composite material based on copper ferrite, aluminium and graphite carbon nitride prepared according to the method of any one of claims 1-5 as a nano thermite.
7. Use of a high energy composite material based on copper ferrite, aluminum and graphite carbon nitride prepared according to the method of any one of claims 1-5 as an energetic material thermal decomposition catalyst.
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