CN110937965A - Preparation method and application of high-energy composite material copper ferrite/GO/Al - Google Patents

Preparation method and application of high-energy composite material copper ferrite/GO/Al Download PDF

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CN110937965A
CN110937965A CN201911221808.1A CN201911221808A CN110937965A CN 110937965 A CN110937965 A CN 110937965A CN 201911221808 A CN201911221808 A CN 201911221808A CN 110937965 A CN110937965 A CN 110937965A
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徐抗震
王敬华
王为民
杨燕京
赵凤起
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Abstract

The invention relates to a preparation method and application of a high-energy composite material copper ferrite/GO/Al, wherein a graphene oxide suspension, an aluminum powder suspension and a copper ferrite suspension are respectively prepared. Then dividing GO suspension into two parts, respectively adding the two parts into aluminum powder suspension and copper ferrite suspension for ultrasonic treatment, mixing the two parts for ultrasonic treatment, and finally performing centrifugal drying to obtain CuFe2O4(ii)/GO/Al. The high-energy composite material copper ferrite/GO/Al prepared by the invention has metal composite oxides and metal fuels, can generate sustainable violent redox reaction, and releases huge energy; can be used as combustion catalyst of solid propellant, and has better catalytic effect on the thermal decomposition of energetic materials (such as RDX) than that of single-component CuFe2O4The quick steady-state combustion of the solid propellant is realized, and the pressure index is reduced. The synthesis method of the inventionThe method is simple and effective, has good environment and is easy for industrial production.

Description

Preparation method and application of high-energy composite material copper ferrite/GO/Al
Technical Field
The invention belongs to the technical field of nano energetic materials, and particularly relates to copper ferrite (CuFe) based on a metal composite oxide2O4) High energy composite CuFe with GO2O4Preparation method of/GO/AlAnd applications.
Background
Aluminum (Al) has a high specific energy density (31kJ g)-1) And earth abundance, and thus can be used as a fuel for solid energetic materials to generate heat, gas and thrust, and is widely used in the fields of space propulsion, pyrotechnics, micro electro mechanical systems, and the like. Nano thermites are generally defined as heterogeneous mixtures of metal fuels (aluminum, boron, magnesium, etc.) and inorganic oxidants (metal oxides) having nanoscale dimensions, with energy densities and reaction rates that are not achievable with traditional micron-sized materials. The nanometer energetic composite material with a certain proportion can generate self-propagating aluminothermic reaction after being ignited by a detonator, finally, alumina and simple substance metal are obtained, a large amount of heat is released, the temperature reaches thousands of ℃, and the nanometer energetic composite material can be used as one of typical energetic materials for a solid rocket propellant. Since the exothermic combustion reaction is a solid state diffusion process, it is desirable to increase the specific surface area of interaction between the two phases of nano-scale fuel and oxidant and to reduce the diffusion distance required for the reaction.
The Graphene Oxide (GO) layer of the two-dimensional sheet material is interacted by strong covalent bonds, and van der Waals force is mainly applied between layers, so that the Graphene Oxide (GO) layer is easy to peel off into a single layer or a plurality of layers of sheets with high specific surface area, a large number of oxygen-containing functional groups such as carboxyl, hydroxyl, epoxy and the like exist on the two-dimensional base plane and the edge of the graphene oxide layer, and the hydroxyl and carboxyl groups on the surface enable the graphene oxide layer to be negatively charged, so that the graphene oxide layer is more easily compounded with positively charged nanoparticles on the surface through long-range electrostatic interaction and van der Waals force, the agglomeration of the nanoparticles is reduced, two phases are uniformly mixed, the optimal phase interface contact is realized.
At present, the solid propellant develops towards the directions of high energy, insensitive feeling, low characteristic signal, environmental protection and the like. Nano metal composite oxides have proven to be particularly advantageous as combustion catalysts. If the nano thermite based on the metal composite oxide is used as a propellant combustion catalyst, the composite material has multiple functions, on one hand, different metals of the metal composite oxide can generate a 'synergistic effect', and the catalytic combustion effect of the composite material is better than that of a single metal oxide; on the other hand, GO has high specific surface area, thermal conductivity and mechanical strength, and can improve the combustion performance of energetic materials (such as RDX); and the nano aluminum powder has strong reaction activity, can obviously improve the energy and the burning speed of the propellant, and can be used as a functional additive of the solid propellant.
Disclosure of Invention
One of the objects of the present invention is to provide a high energy composite material CuFe2O4Preparation method of/GO/Al.
Another object of the present invention is to provide CuFe prepared by the above method2O4the/GO/Al is applied as a nano thermite.
The invention also aims to provide CuFe prepared by the method2O4The application of/GO/Al as a thermal decomposition catalyst of energetic materials (such as RDX).
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the high-energy composite material copper ferrite/GO/Al comprises the steps of adding a GO suspension into an Al powder suspension, and uniformly mixing to obtain a mixed solution A; adding GO suspension to CuFe2O4Uniformly mixing the suspension to obtain a mixed solution B; and uniformly mixing the mixed solution A and the mixed solution B, centrifuging, washing and drying to obtain the high-energy composite material copper ferrite/GO/Al.
A further improvement of the invention is that the GO suspension is made by the following process: adding GO into a solvent, and performing ultrasonic treatment to prepare GO suspension; the Al powder suspension was prepared by the following procedure: adding nano Al into a solvent, and performing ultrasonic treatment to obtain an Al powder suspension; CuFe2O4The suspension was prepared by the following procedure: mixing nano CuFe2O4Adding the mixture into a solvent for ultrasonic treatment to prepare CuFe2O4And (3) suspension.
The further improvement of the invention is that the grain diameter of the nano Al is 80-300 nm.
The invention is further improved in that the nano CuFe2O4The particle size of (D) is 150-300 nm.
The invention further improves that the solvent is N, N-dimethylformamide and/or isopropanol;
the invention has the further improvement that the ultrasonic time is 1h-4 h.
The further improvement of the invention is that the GO in the high-energy composite material copper ferrite/GO/Al accounts for 1-2.5% by mass.
The invention is further improved in that Al and CuFe2O4The molar ratio of (2.3-6.7) to (1).
The application of the high-energy composite material copper ferrite/GO/Al prepared by the method as a nano thermite.
The application of the high-energy composite material copper ferrite/GO/Al prepared by the method as a thermal decomposition catalyst of an energy-containing material. Compared with the prior art, the invention has the following beneficial effects:
(1) the high-energy composite material CuFe prepared by the invention2O4/GO/Al with metal complex oxides (CuFe)2O4) And metal fuel (Al), which can undergo sustainable vigorous redox reactions and release enormous energy; meanwhile, the metal composite oxide CuFe2O4More oxygen can be provided for the redox reaction of the composite material, so that the energy release is further improved; GO is a transparent ultrathin layer with 2-3 nm, the surface of GO is negatively charged by oxygen-containing functional groups, and the positive charged Al and CuFe are charged by electrostatic action2O4The uniform load has increased two-phase area of contact on the GO surface, reduces the reunion, and the dispersion is even, realizes the orderly equipment, is favorable to the combined material fully to react.
(2) The synthetic method is simple and effective, is environment-friendly and is easy for industrial production; CuFe synthesized by the invention2O4the/GO/Al can be used as a combustion catalyst of a solid propellant, and the catalytic effect on the thermal decomposition of energetic materials (such as RDX) is better than that of single-component CuFe2O4The quick steady-state combustion of the solid propellant is realized, and the pressure index is reduced.
Drawings
FIG. 1 is CuFe of example 12O4SEM and TEM images of/GO/Al; wherein (a) is CuFe2O4SEM picture of (1); (b) SEM picture of GO; (c)SEM picture of Al; (d) is CuFe2O4SEM picture of/GO/Al, (e) CuFe2O4TEM image of/GO/Al.
FIG. 2 is CuFe of example 12O4XRD profile of/GO/Al;
FIG. 3 is CuFe of examples 1-42O4XRD profile of/GO/Al;
FIG. 4 is CuFe2O4DSC plot of/GO/Al;
FIG. 5 is a DSC plot of the thermal decomposition of RDX in the presence of different catalysts.
Detailed Description
The following are specific examples provided by the inventors to further explain the technical solutions of the present invention.
High-energy composite material CuFe2O4The preparation method of/GO/Al comprises the following steps: firstly, respectively preparing a Graphene Oxide (GO) suspension, a nano aluminum powder (Al) suspension and nano copper ferrite (CuFe)2O4) A suspension;
GO suspension is made by the following process: adding GO into a solvent, and performing ultrasonic treatment to prepare GO suspension;
the Al powder suspension was prepared by the following procedure: adding nano Al into a solvent, and performing ultrasonic treatment to obtain an Al powder suspension;
CuFe2O4the suspension was prepared by the following procedure: mixing nano CuFe2O4Adding the mixture into a solvent for ultrasonic treatment to prepare CuFe2O4And (3) suspension.
Then adding GO suspension into Al powder suspension and CuFe respectively according to a certain proportion2O4Performing ultrasound in the suspension; mixing the two obtained mixed solutions, continuously performing ultrasonic treatment, and finally performing centrifugal washing and drying to obtain CuFe2O4the/GO/Al product.
The grain diameter of the nano Al is 80-300nm, and the nano CuFe2O4The particle size of (D) is about 150-300 nm.
The solvent used in the preparation of the suspension in the present invention is N, N-Dimethylformamide (DMF) and/or isopropanol; when a mixed solution of N, N-dimethylformamide and isopropanol is used, the volume ratio of the two may be any ratio.
The ultrasonic time is as follows: 1h-4 h; the GO is CuFe2O41% to 2.5% (wt)/GO/Al weight; al and CuFe when the equivalence ratio (phi) is 1-2.52O4The amount ratio of the substances of (a) is 2.3:1 to 6.7: 1.
Wherein the equivalence ratio Φ can be defined as:
Figure BDA0002301055040000041
wherein n (fuel) is the amount of Al and n (oxidazer) is CuFe2O4The numerator represents the actual amount used and the denominator represents the stoichiometry.
CuFe2O4the/GO/Al is applied as a nano thermite.
CuFe2O4The application of/GO/Al as a thermal decomposition catalyst of energetic materials (such as RDX).
Example 1
(1) Dispersing GO (25.0mg) in 25mL of N, N-Dimethylformamide (DMF) solution, and carrying out ultrasonic treatment for 3h to obtain GO suspension;
(2) according to Al and CuFe2O4The thermite reaction that occurs calculates the stoichiometric ratio of fuel to oxidant, whose equivalence ratio Φ can be defined as:
Figure BDA0002301055040000051
wherein n (fuel) is the amount of fuel material, n (oxidizer) is the amount of oxidant material,
n (CuFe) according to the equivalent ratio phi of 2.0[ n (Al) ]2O4)＝5.3:1]Al and CuFe are obtained by calculation2O4The amount (n) and mass (m) of the substance(s) are 368.0mg of nano Al powder (purity 99.5%) and 608.9mg of CuFe2O4Dispersing in 50mL of mixed solution of N, N-Dimethylformamide (DMF) and Isopropanol (IPA) (DMF: IPA volume ratio is 1:1) respectively, and performing ultrasonic treatment for 3h to prepare nano Al suspension and nano CuFe2O4A suspension;
(3) the GO suspension prepared in the step (1) is averagely divided into two parts (12.5mL) and respectively added into the Al suspension prepared in the step (2) and CuFe2O4Performing ultrasonic treatment for 1h in the suspension to uniformly mix and disperse the suspension to obtain a mixed solution A and a mixed solution B;
(4) and (4) mixing the mixed solution A and the mixed solution B obtained in the step (3) again, and continuing to perform ultrasonic treatment for 2 h.
(5) Centrifugally washing and drying to obtain the high-energy composite CuFe2O4and/GO/Al (phi is 2.0). High-energy composite material CuFe2O4The GO content in/GO/Al is 2.5% wt.
FIG. 1 shows CuFe prepared in this example2O4SEM image of/GO/Al (a: CuFe)2O4；b:GO；c:Al；d:CuFe2O4/GO/Al) and TEM images (e: CuFe)2O4/GO/Al), the results show that: nano CuFe with rough surface2O4The particles (a) and the nano Al particles (c) with smooth surfaces are uniformly mixed and relatively uniformly loaded on the surface of GO, so that the contact area of two phases is increased. The sample combustion heat was 11284J g-1。
FIG. 2 shows CuFe prepared in this example2O4XRD pattern of/GO/Al, the result shows that: CuFe2O4Diffraction peak and CuFe of XRD curve of/GO/Al2O4The standard cards of (JCPDS No. 77-0010) and Al (JCPDS No. 04-0787) are in agreement, the peak at 2 θ ═ 9.54 ° corresponds to the characteristic peak of GO, indicating that graphene oxide is exfoliated to form single or multilayer ultrathin sheets, and Al and CuFe2O4Successfully loaded onto the surface of a thin GO layer.
Example 2
(1) Dispersing GO (25.0mg, 2.5% wt) in 25mL of N, N-Dimethylformamide (DMF) solution, and performing ultrasonic treatment for 2h to obtain GO suspension; n (CuFe) according to the equivalent ratio phi of 1.4[ n (Al) ]2O4)＝3.7:1]290.3mg of Al (99.5% purity) and 686.2mg of CuFe were weighed out2O4Dispersing in 50mL Isopropanol (IPA) solution respectively, and performing ultrasonic treatment for 2h to prepare nano Al suspension and nano CuFe2O4A suspension;
(2) dividing the GO suspension prepared in the step (1) into two equal parts (12.5mL) to be respectively added into the Al suspension and the CuFe2O4Carrying out ultrasonic treatment on the suspension for 1h to uniformly mix and disperse the suspension to obtain a mixed solution A and a mixed solution B;
(3) and (3) mixing the mixed solution A and the mixed solution B in the step (2) again, and continuing to perform ultrasonic treatment for 2 h.
(4) Centrifugally washing and drying to obtain the high-energy composite CuFe2O4and/GO/Al (phi is 1.4). The combustion heat is 9035J g-1。
Example 3
(1) Dispersing GO (25.0mg, 2.5% wt) in 50mL of N, N-Dimethylformamide (DMF) solution, and performing ultrasonic treatment for 4h to obtain GO suspension; n (CuFe) according to the equivalent ratio phi of 1.8[ n (Al) ]2O4)＝4.8:1]344.1mg of nano Al (purity 99.5%) and 632.5mg of nano CuFe are weighed2O4Dispersing in 50mL Isopropanol (IPA) solution respectively, and performing ultrasonic treatment for 2h to prepare nano Al suspension and nano CuFe2O4A suspension;
(2) dividing the GO suspension prepared in the step (1) into two equal parts (12.5mL) to be respectively added into the Al suspension and the CuFe2O4Carrying out ultrasonic treatment on the suspension for 2 hours to uniformly mix and disperse the suspension to obtain a mixed solution A and a mixed solution B;
(3) and (3) mixing the mixed solution A and the mixed solution B in the step (2) again, and continuing to perform ultrasonic treatment for 3 hours.
(4) Centrifugally washing and drying to obtain the high-energy composite CuFe2O4and/GO/Al (phi is 1.8). The heat of combustion is 11040J g-1。
Example 4
(1) Dispersing GO (25.0mg, 2.5% wt) in 25mL of N, N-Dimethylformamide (DMF) solution, and performing ultrasonic treatment for 4h to obtain GO suspension; n (CuFe) according to the equivalent ratio phi of 2.5[ n (Al) ]2O4)＝6.7:1]420.5mg of Al (99.5% purity) and 556.5mg of CuFe were weighed out2O4Dispersing in 50mL of mixed solution of N, N-Dimethylformamide (DMF) and Isopropanol (IPA) (volume ratio DMF: IPA 1:1) respectively, and performing ultrasonic treatment for 4h to prepare nano Al suspension and nano CuFe2O4A suspension;
(2) dividing the GO suspension prepared in the step (1) into two equal parts (12.5mL) to be respectively added into the Al suspension and the CuFe2O4Carrying out ultrasonic treatment on the suspension for 2 hours to uniformly mix and disperse the suspension to obtain a mixed solution A and a mixed solution B;
(3) and (3) mixing the mixed solution A and the mixed solution B in the step (2) again, and continuing to perform ultrasonic treatment for 3 hours.
(4) Centrifugally washing and drying to obtain the high-energy composite CuFe2O4GO/Al (Φ 2.5). Its combustion heat is 12785J g-1。
FIG. 3 is a graph of CuFe prepared in examples 1-42O4XRD pattern of/GO/Al, the result shows that: CuFe2O4Diffraction peaks of XRD curve of/GO/Al are both equal to CuFe2O4Standard cards of (JCPDS No. 77-0010) and Al (JCPDS No. 04-0787) were identical, and CuFe2O4And the peak intensity of Al corresponds to the equivalent ratio of the two.
DSC test:
taking the high-energy composite CuFe synthesized by the method of the embodiment 1 to 42O4(phi ═ 1.4, 1.8, 2.0, and 2.5) at a temperature rise rate of 10 ℃ for min-1DSC measurement is carried out under the condition, the result shown in figure 4 is obtained, and the high-energy composite material Al/CuFe2O4the/GO is decomposed at about 610 ℃, and the heat release amounts are 1454, 1740, 2172 and 2116J g-1And the heat release amount thereof reaches the maximum when Φ is 2.0.
DSC test after mixing with RDX:
high energy composite CuFe synthesized by the methods of examples 1-42O4(ii)/GO/Al with RDX at 1: 4, and heating at a temperature rising rate of 10 ℃ for min-1DSC measurement was carried out under the conditions shown in FIG. 5. The melting peak-to-peak temperature of RDX is not obviously changed, the pure RDX decomposition peak temperature is 240.3 ℃, and GO/Al/CuFe corresponding to different phi values2O4The peak temperature of the main peak of RDX is respectively reduced by 5.4 ℃, 4.6 ℃ and 3.4 ℃, and the apparent activation energy of decomposition is reduced by 26.3kJ mol compared with that of pure RDX when phi is 2.0-1Has obvious catalytic decomposition effect.
Example 5
The Al powder suspension was prepared by the following procedure: adding nano Al with the particle size of 80-300nm into N, N-dimethylformamide, and carrying out ultrasonic treatment for 2h to prepare an Al powder suspension;
GO suspension is made by the following process: adding GO into N, N-dimethylformamide, and carrying out ultrasonic treatment for 1h to obtain a GO suspension;
CuFe2O4the suspension was prepared by the following procedure: nano CuFe with the grain diameter of 150-300nm2O4Adding the mixture into N, N-dimethylformamide for ultrasonic treatment for 3 hours to prepare CuFe2O4And (3) suspension.
Equally dividing the GO suspension into two parts, adding one part of GO suspension into the Al powder suspension, uniformly mixing to obtain a mixed solution A, and adding the other part of GO suspension into CuFe2O4Uniformly mixing the suspension to obtain a mixed solution B; al and CuFe2O4The molar ratio of the mixed solution A to the mixed solution B is 5.3:1, the mixed solution A and the mixed solution B are uniformly mixed, and the mixture is centrifuged, washed and dried to obtain the high-energy composite material copper ferrite/GO/Al. Wherein the weight fraction of GO in the high-energy composite material copper ferrite/GO/Al is 1.5%.
Example 6
The Al powder suspension was prepared by the following procedure: adding nano Al with the particle size of 80-300nm into isopropanol, and carrying out ultrasonic treatment for 2h to prepare an Al powder suspension;
GO suspension is made by the following process: adding GO into isopropanol, and performing ultrasonic treatment for 1h to obtain GO suspension;
CuFe2O4the suspension was prepared by the following procedure: nano CuFe with the grain diameter of 150-300nm2O4Adding into isopropanol, and performing ultrasonic treatment for 3h to obtain CuFe2O4And (3) suspension.
Equally dividing the GO suspension into two parts, adding one part of GO suspension into the Al powder suspension, uniformly mixing to obtain a mixed solution A, and adding the other part of GO suspension into CuFe2O4Uniformly mixing the suspension to obtain a mixed solution B; al and CuFe2O4The molar ratio of the mixed solution A to the mixed solution B is 5.3:1, the mixed solution A and the mixed solution B are evenly mixed, centrifuged, washed and dried to obtain the high-energy composite materialCopper ferrite/GO/Al. Wherein the weight fraction of GO in the high-energy composite material copper ferrite/GO/Al is 1%.
Example 7
The Al powder suspension was prepared by the following procedure: adding nano Al with the particle size of 80-300nm into N, N-dimethylformamide, and carrying out ultrasonic treatment for 2h to prepare an Al powder suspension;
GO suspension is made by the following process: adding GO into a mixed solution of N, N-dimethylformamide and isopropanol, and carrying out ultrasonic treatment for 1h to obtain a GO suspension; wherein the volume ratio of the N, N-dimethylformamide to the isopropanol is 1: 1.
CuFe2O4The suspension was prepared by the following procedure: nano CuFe with the grain diameter of 150-300nm2O4Adding the mixture into N, N-dimethylformamide for ultrasonic treatment for 3 hours to prepare CuFe2O4And (3) suspension.
Equally dividing the GO suspension into two parts, adding one part of GO suspension into the Al powder suspension, uniformly mixing to obtain a mixed solution A, and adding the other part of GO suspension into CuFe2O4Uniformly mixing the suspension to obtain a mixed solution B; al and CuFe2O4The molar ratio of the mixed solution A to the mixed solution B is 2.3:1, the mixed solution A and the mixed solution B are uniformly mixed, and the mixture is centrifuged, washed and dried to obtain the high-energy composite material copper ferrite/GO/Al. Wherein the weight fraction of GO in the high-energy composite material copper ferrite/GO/Al is 2.5%.
CuFe prepared by the method2O4The application of/GO/Al as a nano thermite; can also be used as a combustion catalyst of solid propellant.
The invention relates to a high-energy composite CuFe material prepared by electrostatic assembly2O4the/GO/Al is a metal composite oxide (CuFe)2O4) And the GO is added to enable the two phases to be uniformly mixed, the heat release is improved, and meanwhile, the GO has excellent electrical conductivity and large specific surface area, so that the catalytic combustion effect of the GO on a solid propellant is further enhanced.

Claims (10)

1. The preparation method of the high-energy composite material copper ferrite/GO/Al is characterized in that GO suspension is preparedAdding the mixture into the Al powder suspension, and uniformly mixing to obtain a mixed solution A; adding GO suspension to CuFe2O4Uniformly mixing the suspension to obtain a mixed solution B; and uniformly mixing the mixed solution A and the mixed solution B, centrifuging, washing and drying to obtain the high-energy composite material copper ferrite/GO/Al.
2. The method for preparing high-energy composite copper ferrite/GO/Al according to claim 1, wherein the GO suspension is prepared by the following process: adding GO into a solvent, and performing ultrasonic treatment to prepare GO suspension; the Al powder suspension was prepared by the following procedure: adding nano Al into a solvent, and performing ultrasonic treatment to obtain an Al powder suspension; CuFe2O4The suspension was prepared by the following procedure: mixing nano CuFe2O4Adding the mixture into a solvent for ultrasonic treatment to prepare CuFe2O4And (3) suspension.
3. The method for preparing the high-energy composite material of copper ferrite/GO/Al according to claim 2, wherein the particle size of the nano Al is 80-300 nm.
4. The method for preparing the high-energy composite material copper ferrite/GO/Al according to claim 2, wherein the nano CuFe2O4The particle size of (D) is 150-300 nm.
5. The method for preparing the high-energy composite material of copper ferrite/GO/Al according to claim 2, wherein the solvent is N, N-dimethylformamide and/or isopropanol.
6. The method for preparing the high-energy composite material copper ferrite/GO/Al according to claim 2, wherein the ultrasonic time is 1-4 h.
7. The method for preparing the high-energy composite material copper ferrite/GO/Al according to claim 1, wherein the mass content of GO in the high-energy composite material copper ferrite/GO/Al is 1% -2.5%.
8. The method for preparing the high-energy composite material of copper ferrite/GO/Al according to claim 1, wherein Al and CuFe2O4The molar ratio of (2.3-6.7) to (1).
9. Use of high energy composite copper ferrite/GO/Al prepared according to the method of any one of claims 1-8 as a nano thermite.
10. Use of high energy composite copper ferrite/GO/Al prepared according to the method of any one of claims 1 to 8 as a catalyst for thermal decomposition of energetic materials.
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CN115282994A (en) * 2022-07-04 2022-11-04 西北大学 Preparation method and application of high-energy composite material based on copper ferrite, aluminum and graphite carbon nitride

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