CN114410147A - Preparation method of nano thermite energetic printing ink - Google Patents
Preparation method of nano thermite energetic printing ink Download PDFInfo
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- CN114410147A CN114410147A CN202111606422.XA CN202111606422A CN114410147A CN 114410147 A CN114410147 A CN 114410147A CN 202111606422 A CN202111606422 A CN 202111606422A CN 114410147 A CN114410147 A CN 114410147A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003832 thermite Substances 0.000 title claims abstract description 12
- 238000007639 printing Methods 0.000 title claims description 14
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 32
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 32
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000005751 Copper oxide Substances 0.000 claims abstract description 25
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 25
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 23
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 5
- 238000001248 thermal gelation Methods 0.000 claims abstract description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 239000010949 copper Substances 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 22
- 238000001132 ultrasonic dispersion Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000002360 explosive Substances 0.000 description 4
- 239000007800 oxidant agent Substances 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 238000011960 computer-aided design Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 238000001652 electrophoretic deposition Methods 0.000 description 1
- 238000007590 electrostatic spraying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/14—Printing inks based on carbohydrates
Abstract
The invention discloses a preparation method of nano aluminum/porous copper oxide ink. The method comprises two stages, the first stage is to adopt Cu (NO)3)2·H2And O and urea obtain a copper oxide precursor, then calcining the copper oxide precursor at high temperature in a muffle furnace to obtain sheet-shaped porous copper oxide, and then physically mixing the porous copper oxide pCuO with nAl powder to obtain the nAl/pCuO energetic composite material. The second stage is an ink preparation stage, firstly, fully stirring hydroxypropyl methylcellulose HPMC in DMF to completely dissolve the HPMC, then adding the obtained nAl/pCuO energetic composite material into the HPMC solution, and obtaining the nAl/pCuO/HPMC energetic ink after magnetic stirring and thermal gelation. The energy-containing ink prepared by the invention increases the contact area between the nano aluminum powder and the copper oxide, and has a promoting effect on improving the energy release and the reaction performance of the nano thermite. At the same time, the nano thermite is prepared by adding a binderThe suspension type ink is prepared, so that the application of the suspension type ink is expanded.
Description
Technical Field
The invention belongs to the technical field of preparation of energetic materials, and relates to a preparation method of nano thermite energetic ink.
Background
In the early 21 st century, nano metal powder (Al, Mg, etc.) and metal oxide (CuO, Pb, etc.) were used due to excellent heat release characteristics3O4Etc.), fluoride and other oxidants, and the two-component or multi-component energy-containing metastable-state composite material with a fine structure prepared by mixing the oxidants, such as fluoride, gradually enters the field of people and is widely applied to the military fields of explosives, propellants, reaction fragments and the like. However, with the development of the MEMS initiating explosive device technology, the traditional processing method cannot satisfy the high integration of the metastable energetic composite material on the micro initiating explosive device system.
At present, methods for integrating the metastable energetic composite material with initiating explosive devices include magnetron sputtering, electrophoretic deposition, electrostatic spraying and the like, but the methods have high cost and are not suitable for mass production. The ink direct-writing forming technology is a non-mold forming method integrating computer aided design, precision machinery and materials science, a CAD program can be written in advance through a computer, and then the materials are stacked layer by layer on a substrate through a three-dimensional numerical control platform. The method has the advantage of carrying out batch treatment on the material in a micro size, does not need high-temperature and high-pressure treatment, and greatly enhances the applicability of the nano thermite.
The preparation of the ink is crucial to the reactivity and the forming effect of the energetic material. Energy-containing inks are generally composed of a binder, an energy-containing composite material, and a solvent. Too much binder can reduce the sensitivity of the energetic material during the design of the ink formulation, and too little binder can affect the formability of the material on the substrate and can easily block the needle during printing. There is therefore a need to develop energetic inks with moderate viscosity, shear thinning behavior, and high solids content.
Disclosure of Invention
The invention aims to provide a preparation method of nano thermite energetic printing ink. The method adopts nano aluminum powder and porous copper oxide as an energy-containing composite material, HPMC as a binder and DMF as a solvent. The contact area between the fuel and the oxidant can be effectively increased, the reaction performance is improved, and the printing adaptability is good.
The technical scheme for realizing the purpose of the invention is as follows:
the preparation method of the nAl/pCuO/HPMC energetic ink comprises the following steps:
step 1: the porous copper oxide precursor is prepared by a hydrothermal synthesis method by using copper nitrate trihydrate and urea as raw materials.
Step 2: and (3) calcining the copper oxide precursor at high temperature to obtain the flaky porous copper oxide.
And step 3: firstly, the porous copper oxide is dispersed in isopropanol by ultrasound, and then the nano aluminum powder is added for ultrasound mixing. And carrying out suction filtration and drying on the suspension to obtain the nAl/pCuO energetic composite material.
And 4, step 4: hydroxypropyl methylcellulose (HPMC) was dissolved in DMF and stirred to obtain a homogeneous HPMC solution.
And 5: the nAl/pCuO energetic composite material is added into the HPMC solution, and the nAl/pCuO/HPMC energetic printing ink can be obtained through stirring and thermal gelation processes.
Preferably, the temperature of the hydrothermal synthesis is 100-150 ℃, and the reaction time is 3-6 h.
Preferably, the calcining temperature is 500-600 ℃, and the calcining time is 3-10 h.
Preferably, the dosage of the isopropanol is 50-100 mL, and the ultrasonic mixing time is 10-60 min.
Preferably, the equivalent ratio of the nano aluminum powder to the porous copper oxide is 1-2.
Preferably, the activity of the nano aluminum powder is 60-75%.
Preferably, the amount of DMF is 3-5 mL.
Preferably, the volume ratio of the HPMC to the solvent is 0.016-0.03 g/mL, and the ratio of the mass of the nAl/pCuO nano thermite to the volume of the printing ink is 0.3-0.31 g/mL.
Preferably, the temperature of the gelation process is 60 to 100 ℃.
Compared with the prior art, the invention has the following advantages:
(1) the contact area between the flaky porous copper oxide and the nano aluminum powder can be increased, and the reactivity of the nano thermite is improved; (2) the flaky porous structure of the oxidant can reduce the agglomeration phenomenon among particles to a certain extent (3) HPMC with thermal gelation property is used as a binder, the nano thermite can be prepared into energetic printing ink with moderate viscosity under the condition of low binder content, the preparation method is simple, and the method is suitable for direct writing and forming of the printing ink.
Drawings
FIG. 1 is an SEM image of nAl/pCuO/HPMC energetic ink of example 1.
FIG. 2 is a DSC plot of nAl/pCuO/HPMC energetic ink of example 1.
FIG. 3 is a high speed photographic image of nAl/pCuO/HPMC energetic ink of example 1 on a nichrome wire fire bridge.
Detailed Description
The invention is further illustrated by the following examples and figures:
example 1
Step 1: 1.208g of copper nitrate trihydrate and 0.3g of urea were dissolved in 50mL of deionized water and stirred for 30 min.
Step 2: and (3) pouring the solution obtained in the step (1) into a high-pressure hydrothermal kettle for hydrothermal synthesis, wherein the reaction temperature is 130 ℃, and the reaction time is 4 hours.
And step 3: and filtering, washing with deionized water, washing with absolute ethyl alcohol and drying the product of the hydrothermal synthesis to obtain the porous copper oxide precursor.
And 4, step 4: and calcining the precursor by using a muffle furnace, wherein the calcining temperature is 500 ℃, and the calcining time is 4 h.
And 5: adding the porous copper oxide into 50mL of isopropanol, performing ultrasonic dispersion for 40min, then adding the nano aluminum powder, performing ultrasonic dispersion for 40min, and finally performing magnetic stirring for 12 h.
Step 6: and (5) carrying out suction filtration, washing and drying on the suspension subjected to ultrasonic dispersion in the step 5 to obtain the nAl/pCuO energetic composite material.
And 7: 0.05g HPMC is weighed out in 3mL DMF and stirred magnetically for 2 h.
And 8: and (3) adding 0.95g of the nAl/pCuO energetic composite material obtained in the step (6) into the HPMC solution, stirring for 24 hours, and preserving the temperature at 70 ℃ for 10min to obtain the nAl/pCuO/HPMC energetic printing ink with moderate viscosity.
FIG. 1 is an SEM image of an energy-containing ink, and it can be seen from the SEM image that copper oxide is in a porous flake shape, and nano aluminum powder and copper oxide are uniformly compounded. FIG. 2 is a DSC curve of an energy-containing ink, under the test conditions: in Ar atmosphere, the heating rate is 20K/min, the temperature range is 25-1000 ℃, and the gas speed is 30 mL/min. FIG. 3 is a high speed photographic image of energetic ink firing on a nickel chromium wire ignition bridge.
Example 2
Step 1: 12.08g of copper nitrate trihydrate and 3.003g of urea were dissolved in 500mL of deionized water and stirred for 30 min.
Step 2: and (3) pouring the solution obtained in the step (1) into a high-pressure hydrothermal kettle for hydrothermal synthesis, wherein the reaction temperature is 130 ℃, and the reaction time is 4 hours.
And step 3: and filtering, washing with deionized water, washing with absolute ethyl alcohol and drying the product of the hydrothermal synthesis to obtain the porous copper oxide precursor.
And 4, step 4: and calcining the precursor by using a muffle furnace, wherein the calcining temperature is 500 ℃, and the calcining time is 4 h.
And 5: adding the porous copper oxide into 50mL of isopropanol, performing ultrasonic dispersion for 60min, then adding the nano aluminum powder, performing ultrasonic dispersion for 60min, and finally performing magnetic stirring for 12 h.
Step 6: and (5) carrying out suction filtration, washing and drying on the suspension subjected to ultrasonic dispersion in the step 5 to obtain the nAl/pCuO energetic composite material.
And 7: 0.06g of HPMC is weighed into 3mL of DMF and stirred magnetically for 2 h.
And 8: and (3) adding 0.94g of the nAl/pCuO energetic composite material obtained in the step (6) into the HPMC solution, stirring for 24 hours, and preserving the temperature at 70 ℃ for 10 minutes to obtain the nAl/pCuO/HPMC energetic printing ink with moderate viscosity.
Example 3
Step 1: 24.16g of copper nitrate trihydrate and 6.006g of urea were dissolved in 500mL of deionized water and stirred for 30 min.
Step 2: and (3) pouring the solution obtained in the step (1) into a high-pressure hydrothermal kettle for hydrothermal synthesis, wherein the reaction temperature is 130 ℃, and the reaction time is 5 hours.
And step 3: and filtering, washing with deionized water, washing with absolute ethyl alcohol and drying the product of the hydrothermal synthesis to obtain the porous copper oxide precursor.
And 4, step 4: and calcining the precursor by using a muffle furnace, wherein the calcining temperature is 500 ℃, and the calcining time is 5 h.
And 5: adding the porous copper oxide into 50mL of isopropanol, performing ultrasonic dispersion for 40min, then adding the nano aluminum powder, performing ultrasonic dispersion for 40min, and finally performing magnetic stirring for 12 h.
Step 6: and (5) carrying out suction filtration, washing and drying on the suspension subjected to ultrasonic dispersion in the step 5 to obtain the nAl/pCuO energetic composite material.
And 7: 0.07g of HPMC is weighed into 3mL of DMF and stirred magnetically for 2 h.
And 8: and (3) adding 0.93g of the nAl/pCuO energetic composite material obtained in the step (6) into the HPMC solution, stirring for 24 hours, and preserving the temperature at 70 ℃ for 10 minutes to obtain the nAl/pCuO/HPMC energetic printing ink with moderate viscosity.
Claims (9)
1. A preparation method of nano thermite energetic printing ink is characterized by comprising the following steps:
step 1: preparing a porous copper oxide precursor by using copper nitrate trihydrate and urea as raw materials through a hydrothermal synthesis method;
step 2: calcining the copper oxide precursor at high temperature to obtain flaky porous copper oxide;
and step 3: firstly, the porous copper oxide is dispersed in isopropanol by ultrasound, and then the nano aluminum powder is added for ultrasound mixing. Filtering and drying the suspension to obtain the nAl/pCuO energetic composite material;
and 4, step 4: dissolving hydroxypropyl methylcellulose HPMC in DMF, and stirring to obtain uniform clear HPMC solution;
and 5: the nAl/pCuO energetic composite material is added into the HPMC solution, and the nAl/pCuO/HPMC energetic printing ink can be obtained through magnetic stirring and thermal gelation.
2. The preparation method according to claim 1, wherein in the step 1, the temperature of the hydrothermal synthesis is 100-150 ℃ and the reaction time is 3-6 h.
3. The preparation method according to claim 1, wherein in the step 2, the calcination temperature of the precursor is 500-600 ℃, and the calcination time is 3-10 h.
4. The preparation method according to claim 1, wherein in the step 3, the dosage of the isopropanol is 50-100 mL, and the ultrasonic mixing time is 10-60 min.
5. The preparation method according to claim 1, wherein in the step 3, the equivalent ratio of the nano aluminum powder to the porous copper oxide is 1-2.
6. The preparation method according to claim 1, wherein in the step 3, the activity of the nano aluminum powder is 60-75%.
7. The preparation method according to claim 1, wherein in step 4, the ratio of the mass of HPMC to the volume of solvent is 0.016-0.03 g/mL.
8. The preparation method according to claim 1, wherein in step 5, the ratio of the mass of the nAl/pCuO nano thermite in the ink to the volume of the ink is 0.3-0.31 g/mL.
9. The method according to claim 1, wherein the temperature during the thermal gelation process in the step 5 is 60 to 100 ℃.
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- 2021-12-26 CN CN202111606422.XA patent/CN114410147A/en active Pending
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