Energy-releasing composite material and method for manufacturing same

Patent metadata

Field	Value
Publication number	US-12559443-B2
Application number	US-202017602829-A
Country	US
Kind code	B2
Filing date	Apr 9, 2020
Priority date	Apr 9, 2019
Publication date	Feb 24, 2026
Grant date	Feb 24, 2026

Abstract

The invention relates to an energy-releasing composite material comprising at least one nanoporous material and at least one inorganic oxidant, characterised in that said nanoporous material is a nanoporous carbon material.

First claim

The invention claimed is:

1 . Composite energetic material comprising at least one nanoporous material and at least one inorganic oxidiser, characterised in that said nanoporous material is a nanoporous carbonaceous material, said composite energetic material has a decomposition initiation temperature on a thermogram obtained by differential scanning calorimetry of less than 5° C./minute in a closed crucible (DSC peak start temperature) preferably from 50° C. to 200° C., more preferably from 100° C. to 150° C., relative to the decomposition initiation temperature on the DSC thermogram of the inorganic oxidiser, and has at least 30% of the porosity occupied by said inorganic oxidiser, and at most 90% of the porosity occupied by said inorganic oxidiser, said energetic material having an impact sensitivity of at least 2 J,
wherein said nanoporous carbonaceous material comprises a network of interconnected pores in a three-dimensional arrangement of pores which extend through the volume of said nanoporous carbonaceous material,
said nanoporous carbonaceous material comprises micropores with a pore size not exceeding 2 nm, mesopores with an intermediate size of between 2 and 50 nm and macropores with a pore size of greater than 50 nm and less than 100 nm; and
said nanoporous carbonaceous material having a volume of micropores of between 0.1 cm 3 /g and 1.0 cm 3 /g and a volume of mesopores of between 0.05 cm 3 /g and 3.0 cm 3 /g, calculated based on the pore size distribution modelled by 2D-NLDFT-HS (non-linear DFT) or QSDFT (quench-state DFT) applied to nitrogen adsorption isotherms at 77.4K.

2 . Composite energetic material according to claim 1 , having a bulk density greater than or equal to 1.0 g/cm3.

3 . Composite energetic material according to claim 1 , having a micropore volume of pores with a diameter of less than 2 nm of between 0.01 cm3/g and 1.0 cm3/g, calculated by applying the Dubinin-Radushkevitch model applied to nitrogen adsorption isotherms at 77.4K.

4 . Composite energetic material according to claim 1 , comprising a mesopore volume of pores with a diameter of between 2 nm and 50 nm of between 0.05 cm3/g and 3.0 cm3/g, calculated based on the pore size distribution modelled by 2D-NLDFT-HS (2D non-linear DFT HS) or QSDFT (quench-state DFT) applied to nitrogen adsorption isotherms at 77.4K.

5 . Composite energetic material according to claim 1 , wherein said nanoporous carbonaceous material is granular with a D90 greater than or equal to 160 microns and a D10 greater than or equal to 900 microns.

6 . Composite energetic material according to claim 1 , wherein said carbonaceous material is in power form.

7 . Composite energetic material according to claim 6 , wherein the average particle size d50 is between 25 μm and 50 μm.

8 . Composite energetic material according to claim 1 , wherein said carbonaceous material is a monolith.

9 . Composite energetic material according to claim 1 , wherein said inorganic oxidiser is selected from the group of salts of the general formula XaZbOc where a and b are integers between 0 and 5, and where c represents an integer between 1 and 8, with X representing a counter anion selected from Na, K, NH4, Li, H, Ca, Mg, Al or Fe, as well as combinations thereof, with Z representing Mn, Cl, N, S, I, P and O representing oxygen.

10 . Energetic formulation comprising the composite energetic material according to claim 1 .

11 . Energetic formulation according to claim 10 , further comprising at least one conventional additive.

12 . Energetic formulation according to claim 11 , being an explosive energetic formulation or a propellant energetic formulation.

13 . Method of producing a composite energetic material according to claim 1 comprising the following steps:
a) Immersing said at least nanoporous material in said at least one oxidiser present in a fluid;
b) Impregnating said at least one nanoporous material with said at least one oxidiser present in a fluid;
c) Obtaining a composite energetic material
characterised in that said nanoporous material is a nanoporous carbonaceous material; and in that said impregnation step comprises an adsorption of said at least one oxidiser in the micropores, mesopores and macropores forming a core at a temperature of between 0 and 50° C., between 15 and 30° C., preferably between 18 and 28° C., more preferably between 20 and 26° C., said adsorption being followed by a filling of the free micropores, mesopores and macropores by said oxidiser.

14 . Method according to claim 13 , wherein said composite energetic material contains a ratio of the free oxygen atomic fraction of the oxidiser to the carbon contained in the nanoporous carbonaceous material of between 0.5 and 2.5, preferably between 1 and 2.2 and more preferably around 2.

15 . Method according to claim 13 , wherein a minimum carbon content of said nanoporous carbonaceous material included in the composite energetic material according to the present invention is greater than 70% by weight of carbon, preferably greater than 80% by weight of carbon, more preferably greater than 90% by weight of carbon relative to the total weight of said nanoporous carbonaceous material.

16 . Method according to claim 13 , wherein said fluid is a liquid phase comprising said inorganic oxidiser in a solvent.

17 . Method according to claim 16 , wherein said liquid phase is a saturated colloidal solution or suspension of said inorganic oxidiser.

18 . Method according to claim 13 , wherein the filling of the free micropores, mesopores and macropores is performed by evaporation, filtration, vaporisation, extraction, lyophilisation, cryodesiccation or a combination thereof.

19 . Method according to claim 13 , comprising, before obtaining the composite energetic material, a rinsing step with a rinsing solvent and a removal of the rinsing solvent, optionally loaded with excess inorganic oxidiser, by evaporation, filtration, vaporisation, extraction, lyophilisation, cryodesiccation, drying or a combination thereof.

20 . Method according to claim 13 , wherein the nanoporous carbonaceous material is immersed in said fluid under stirring.

21 . Method according to claim 13 , wherein said inorganic oxidiser is selected from the group of salts of the general formula XaZbOc where a and b are integers between 0 and 5, and where c represents an integer between 1 and 8, with X representing a counter anion selected from Na, K, NH4, Li, H, Ca, Mg, Al or Fe as well as combinations thereof, with Z representing Mn, Cl, N, S, P, I and O representing oxygen.

22 . Method according to claim 13 , wherein said nanoporous carbonaceous particles have a micropore volume of pores with a diameter less than or equal to 2 nm of between 0.1 cm3/g and 1.0 cm3/g, calculated by applying the Dubinin-Radushkevitch model applied to a nitrogen adsorption isotherm at 77.4K.

23 . Method according to claim 13 , wherein said nanoporous carbonaceous particles have a mesopore volume of pores with a diameter of between 2 nm and 50 nm of between 0.05 cm3/g and 3.0 cm3/g, calculated based on the pore size distribution modelled by NLDFT (non-linear DFT) or QSDFT (quench-state DFT) applied to a nitrogen adsorption isotherm at 77.4K.

24 . Method according to claim 13 , wherein said nanoporous carbonaceous material is granular, with a D90 greater than or equal to 160 microns and a D10 greater than or equal to 900 microns.

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Assignees

• Ecole Royale Militaire
• Centre Nat Rech Scient

Inventors

• Van Riet Romuald Jean-Pierre
• Ovin Ania Maria Concepcion
• Lefebvre Michel Henri Jean-Marie
• Lodewyckx Peter Jean Joseph

Classifications

• C06B45/04 Primary

  comprising solid particles dispersed in solid solution or matrix {not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive} · CPC title

• C01P2006/16

  Pore diameter · CPC title

• C01P2006/14

  Pore volume · CPC title

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title

• C01B32/15

  Nano-sized carbon materials · CPC title