CN113862755B - Method for improving adhesion of electrophoretic deposited energetic film, improved energetic film and application - Google Patents
Method for improving adhesion of electrophoretic deposited energetic film, improved energetic film and application Download PDFInfo
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- CN113862755B CN113862755B CN202111149334.1A CN202111149334A CN113862755B CN 113862755 B CN113862755 B CN 113862755B CN 202111149334 A CN202111149334 A CN 202111149334A CN 113862755 B CN113862755 B CN 113862755B
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 27
- 238000001652 electrophoretic deposition Methods 0.000 claims abstract description 16
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000011368 organic material Substances 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 8
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 229910052802 copper Inorganic materials 0.000 claims description 15
- 239000010949 copper Substances 0.000 claims description 15
- BPCXHCSZMTWUBW-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F BPCXHCSZMTWUBW-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 19
- 230000001070 adhesive effect Effects 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 12
- 239000000758 substrate Substances 0.000 abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- 238000002791 soaking Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 83
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical group [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 34
- 238000012360 testing method Methods 0.000 description 7
- 244000137852 Petrea volubilis Species 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001962 electrophoresis Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002360 explosive Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003832 thermite Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229920000557 Nafion® Polymers 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
-
- 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
- C06B21/0033—Shaping the mixture
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/04—Electrophoretic coating characterised by the process with organic material
Abstract
The invention discloses a method for improving the adhesive force of an electrophoretic deposition energetic film, which relates to the technical field of energetic materials and comprises the following steps: (1) Adding Al or Mg and metal oxide into an organic solvent according to the mass ratio of 1:1-4, and performing ultrasonic dispersion to obtain a suspension; (2) Adding an organic material into the mixed solution, and performing ultrasonic treatment to obtain a solution; (3) The suspension in the step (1) is used as an electrophoretic deposition solution, a cathode and an anode are placed, and after the power is on, a film is deposited on the surface of the cathode; (4) Immersing the film in the solution obtained in the step (2), standing for 5-30s, and then drying in vacuum. The invention has the beneficial effects that: the invention adopts the solution soaking method to improve the adhesive force of the electrophoretic deposition energetic film on the surface of the substrate, and has the advantages of simple operation flow, low cost, good film stability and strong adhesive force.
Description
Technical Field
The invention relates to the technical field of energetic materials, in particular to a method for improving the adhesive force of an electrophoretic deposited energetic film, an improved energetic film and application thereof.
Background
The thermite is an active reaction substance consisting of a reducing agent (Al, mg, si, B and the like) and an oxidizing agent (metal oxide or non-oxide), can generate a severe oxidation-reduction reaction under the stimulation of external conditions, has high heat value and high adiabatic temperature, can still generate self-propagating in an anaerobic environment in the reaction process, and is widely applied to the fields of combustion agents, ignition agents, high-energy explosive, solid rocket propellants and the like. In recent years, as technologies such as spacecraft and electromechanical initiating explosive devices are developed toward miniaturization and dexterity, thermite film forming technologies are attracting more and more attention.
As a film (or coating) preparation technology, the electrophoresis deposition technology has the advantages of rapid film formation, low requirement on electrode shape (film formation on deep holes or electrode surfaces and inside with complex shapes), low cost and the like, and has important application in the field of energetic materials. Unfortunately, the thin film material prepared by electrophoretic deposition often has the problems of uneven thickness, easy falling off, protrusion and the like, and greatly limits the application range. Therefore, it is important to further study the curing method of the electrophoretic deposition film material to improve the adhesive force of the energetic film. For example, patent application publication No. CN111850655A discloses a method for preparing a high-adhesion nano thermite coating by electrophoretic deposition, but the method needs to adopt an oil phase synthesis method, namely, the synthesis of octadecylamine and nitrate to prepare MOx nano particles, and the preparation method is complex and the process is not easy to control.
Disclosure of Invention
The invention aims to solve the technical problems that the method for improving the electrodeposited film in the prior art is complex, the process is not easy to control, and the method for improving the adhesive force of the electrodeposited energetic film, the improved energetic film and the application are provided.
The invention solves the technical problems by the following technical means:
a method for improving the adhesion of an electrophoretically deposited energetic film comprising the steps of:
(1) Adding Al or Mg and metal oxide into an organic solvent according to the mass ratio of 1:1-4, and performing ultrasonic dispersion to obtain a suspension, wherein the metal oxide is CuO or MoO 3 、Fe 2 O 3 、Cr 2 O 3 、MnO 2 Or Bi 2 O 3 ；
(2) Adding an organic material into the mixed solution, and performing ultrasonic treatment to obtain a solution, wherein the organic material is tridecafluorooctyl triethoxysilane, 1H, 2H-perfluoro decyl triethoxysilane or Nafion perfluorinated resin;
(3) The suspension in the step (1) is used as an electrophoretic deposition solution, a cathode and an anode are placed, and after the power is on, a film is deposited on the surface of the cathode;
(4) Immersing the film in the step (3) into the solution in the step (2), standing for 5-30s, and then drying in vacuum.
The energy-containing film with improved adhesive force prepared by the invention has no other substances except tridecafluorooctyl triethoxysilane, 1H, 2H-perfluoro decyl triethoxysilane or Nafion perfluorinated resin which are loaded in the energy-containing film.
After vacuum drying, the organic solvent is volatilized, and the fluorine-containing organic material contains difunctional groups, so that chemical bonding can be generated between the inorganic particles and hydroxyl, carboxyl and oxygen-containing groups in the base material; in addition, the inert low surface energy groups can provide the treated substrate with very low surface energy and very poor wettability. Meanwhile, in the drying process, particles which are isolated and loosely piled in the cross-linked and solidified film are cross-linked and solidified, so that the compactness of the film and the adhesion force between the film and a substrate are effectively enhanced, and the organic matters are cross-linked and formed into films, and are covered or filled between the particles and a substrate, so that the loose and independently piled particles are solidified and form a whole with the substrate, the physical stability and weather resistance of the film are further improved, and the adhesion force and the hydrophobic capacity of the film on the surface of the substrate are improved. It is noted that the process film particles are only physically mixed with the organic material and no chemical reaction occurs.
The beneficial effects are that: the invention adopts a solution soaking method to improve the adhesive force of the electrophoretic deposition energetic film on the surface of the substrate, and has simple operation flow, low cost, good film stability and strong adhesive force;
the organic material adopted in the invention has the characteristics of combustibility, viscosity, hydrophobicity and the like, and ensures the energy release effect of the energy-containing material while improving the adhesive force of the energy-containing film.
The organic material contains C, H, O, F and other elements, has excellent combustion supporting performance, and is loaded in an energy-containing film system, so that the adhesive force of the energy-containing film is effectively improved, and the combustion and heat release performances of the energy-containing film are improved.
Preferably, the organic solvent in the step (1) is isopropanol, acetone, methanol, ethanol, acetylacetone.
Preferably, the weight fraction of Al or Mg and metal oxide in the organic solvent in the step (1) is 0.1-0.5%.
Preferably, in the step (1), aluminum and copper oxide powder are added into an organic solvent according to a mass ratio of 1:2.
Preferably, the ultrasonic time in the step (1) is not less than 10min, and the ultrasonic temperature is not higher than 30 ℃.
Preferably, the mixed solution in the step (2) is deionized water and absolute ethyl alcohol.
Preferably, in the step (2), tridecafluorooctyl triethoxysilane is dissolved in absolute ethyl alcohol and deionized water to prepare a solution, the concentration of the solution is between 0.1mol/L and 1.0mol/L, and the solution is uniformly mixed by ultrasonic treatment for 10-15 min.
Preferably, in the step (3), the anode and the cathode are polished to be smooth and flat by using 5000-mesh fine sand paper, and are ultrasonically washed by using acetone, ethanol and deionized water for 10 minutes respectively, and then are dried for later use.
Preferably, in the step (3), the electrophoretic deposition voltage is 100-150 v, and the deposition time is not less than 2min.
Preferably, the deposition time is 2-10 min.
Preferably, the cathode and the anode in the step (3) are all pure copper sheets, pure titanium sheets, nickel sheets, iron sheets or stainless steel sheets.
Preferably, the vacuum drying temperature in the step (4) is 80-100 ℃, and the vacuum drying time is 3-5h.
The energetic film obtained by the method is provided.
The beneficial effects are that: the energetic film obtained by the method has good stability and strong adhesive force, and can ensure the energy release effect of the energetic material.
The energetic film obtained by the method is applied to micro-nano energetic devices.
Preferably, the micro-nano energetic device comprises an electromechanical initiating explosive device and an energetic chip.
The invention has the advantages that: the invention adopts a solution soaking method to improve the adhesive force of the electrophoretic deposition energetic film on the surface of the substrate, and has simple operation flow, low cost, good film stability and strong adhesive force;
the organic material adopted in the invention has the characteristics of combustibility, viscosity, hydrophobicity and the like, and ensures the energy release effect of the energy-containing material while improving the adhesive force of the energy-containing film.
The organic material contains C, H, O, F and other elements, has excellent combustion supporting performance, and is loaded in an energy-containing film system, so that the adhesive force of the energy-containing film is effectively improved, and the combustion and heat release performances of the energy-containing film are improved.
Drawings
FIG. 1 is a schematic diagram of an Al/TFs/CuO energetic film in an embodiment of the invention;
in the figure: 1 an organic network layer; 2Al/CuO film layer; 3 copper sheet base material.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Those of skill in the art, without any particular mention of the techniques or conditions, may follow the techniques or conditions described in the literature in this field or follow the product specifications.
Comparative example 1
(1) Adding 100ml of isopropanol into the nano aluminum powder and the copper oxide powder in a mass ratio of 1:2, and carrying out ultrasonic treatment at normal temperature of 40Hz for 10-15 min to prepare a uniform suspension B;
(2) Pure copper sheet (1X 2 cm) 2 ) Polishing with 5000 mesh fine sand paper until the surface is bright and smooth, respectively carrying out ultrasonic treatment with acetone, ethanol and deionized water for 10min, and blow-drying for later use;
(3) Setting the voltage of an electrophoresis apparatus to 150V, setting the deposition time to 5min, using a copper sheet as a cathode and an anode, using a suspension B as an electrolyte, and obtaining a uniform Al/CuO energetic film on a cathode copper sheet;
(4) The resulting Al/CuO energetic film was dried at 60℃under vacuum for 3 h.
The adhesion of the dried Al/CuO film prepared according to the above procedure was evaluated by the scratch "X" test according to film adhesion test Standard ASTM D3359-02. Marking an X symbol on the diagonal line of the film by using a sharp blade, and ensuring that the scratch penetrates through the film to reach the bottom substrate; then, the 3M tape was tightly stuck to the film surface, and then rapidly pulled up. As a result, it was found that the film was severely peeled off in an area exceeding 60%. From the film adhesion rating of 0-5, the unmodified Al/CuO film adhesion rating was about 0B, with very poor adhesion.
Example 1
The preparation method for improving the adhesion of the electrophoretic deposition Al/CuO energetic film comprises the following steps:
(1) Adding 100ml of isopropanol into the nano aluminum powder and the copper oxide powder in a mass ratio of 1:2, and carrying out ultrasonic treatment at normal temperature of 40Hz for 10-15 min to prepare a uniform suspension A;
(2) Polishing the pure copper sheet with 5000 mesh fine sand paper until the surface is bright and smooth, respectively carrying out ultrasonic treatment with acetone, ethanol and deionized water for 10min, and drying for later use;
(3) Adding 0.1ml of tridecafluorooctyl triethoxysilane into 100ml of mixed solution of absolute ethanol and deionized water, and performing ultrasonic treatment for 10min to prepare tridecafluorooctyl triethoxysilane solution A;
(4) Setting the voltage of an electrophoresis apparatus to 150V, setting the deposition time to 5min, using a copper sheet as a cathode and an anode, using a suspension A as an electrolyte, obtaining a uniform Al/CuO energetic film on a cathode copper sheet, and drying for 30h in a vacuum 60 ℃ environment;
(5) Immersing the dried copper sheet loaded with the Al/CuO film into the solution B for 10s;
(6) The Al/CuO film after soaking treatment is dried for 3 hours at the temperature of 70 ℃ in vacuum, the schematic diagram of the obtained energetic film is shown in figure 1, an Al/CuO film layer 2 is attached to a copper sheet substrate 3, and a tridecafluorooctyl triethoxysilane organic network layer 1 is attached to the Al/CuO film layer 2.
(7) According to the film adhesion test standard ASTM D3359-02, the adhesion was initially improved by the 3M tape surface having a small amount of powder adhesion, al/CuO film adhesion rating of about 2B, following the procedure in comparative example 1.
Example 2
The preparation method for improving the adhesion of the electrophoretic deposition Al/CuO energetic film comprises the following steps:
(1) Adding 100ml of isopropanol into the nano aluminum powder and the copper oxide powder in a mass ratio of 1:2, and carrying out ultrasonic treatment at normal temperature of 40Hz for 10-15 min to prepare a uniform suspension B;
(2) Polishing the pure copper sheet with 5000 mesh fine sand paper until the surface is bright and smooth, respectively carrying out ultrasonic treatment with acetone, ethanol and deionized water for 10min, and drying for later use;
(3) Adding 0.5ml of tridecafluorooctyl triethoxysilane into 100ml of mixed solution of absolute ethanol and deionized water, and performing ultrasonic treatment for 10min to prepare tridecafluorooctyl triethoxysilane solution C;
(4) Setting the voltage of an electrophoresis apparatus to 150V, setting the deposition time to 5min, using a copper sheet as a cathode and an anode, using a suspension A as an electrolyte, obtaining a uniform Al/CuO energetic film on a cathode copper sheet, and drying 3h in a vacuum 60 ℃ environment;
(5) Immersing the dried copper sheet loaded with the Al/CuO film into the C solution for 10s;
(6) Drying the Al/CuO film subjected to the soaking treatment for 3 hours at the temperature of 100 ℃ in vacuum;
according to film adhesion test standard ASTM D3359-02, the 3M tape was relatively clean in surface, had little powder adhesion, and had an Al/CuO film adhesion rating of about 3B, with a significant improvement in adhesion, following the procedure in comparative example 1.
Example 3
The preparation method for improving the adhesion of the electrophoretic deposition Al/CuO energetic film comprises the following steps:
(1) Adding 100ml of isopropanol into the nano aluminum powder and the copper oxide powder in a mass ratio of 1:2, and carrying out ultrasonic treatment at normal temperature of 40Hz for 10-15 min to prepare a uniform suspension B;
(2) Polishing the pure copper sheet with 5000 mesh fine sand paper until the surface is bright and smooth, respectively carrying out ultrasonic treatment with acetone, ethanol and deionized water for 10min, and drying for later use;
(3) Adding 0.5ml of tridecafluorooctyl triethoxysilane into 100ml of mixed solution of absolute ethanol and deionized water, and performing ultrasonic treatment for 10min to prepare tridecafluorooctyl triethoxysilane solution D;
(4) Setting the voltage of an electrophoresis apparatus to 150V, setting the deposition time to 5min, using a copper sheet as a cathode and an anode, using a suspension A as an electrolyte, obtaining a uniform Al/CuO film on the surface of a cathode copper sheet, and drying for 3h in a vacuum 60 ℃ environment;
(5) Immersing the dried copper sheet loaded with the Al/CuO film into the D solution for 10s;
(6) Drying the soaked Al/CuO film at the temperature of 100 ℃ in vacuum for 3h;
according to the film adhesion test standard ASTM D3359-02, the test result shows that the 3M adhesive tape has clean surface and no other area on the surface of the film, the Al/CuO film adhesion grade is about 4B, and the adhesion is greatly improved except that a little powder is adhered at the X part.
Example 4
The energetic films of examples 1-4 were tested for heat release by differential scanning calorimeter, and the Al/CuO energetic films loaded with different amounts of tridecafluorooctyltriethoxysilane had heat release values of 1087J/g, 1817J/g, 1977J/g, 2284J/g, respectively. The heat release of the composite film system is improved, and the heat release is increased along with the increase of the concentration of the tridecafluorooctyl triethoxysilane.
Table 1 shows the results of the adhesion rating measurements for the comparative examples and examples
| Examples | Al/CuO | Al/TFs (0.1mol/L)/CuO | Al/TFs (0.5mol/L)/CuO | Al/TFs (1.0mol/L)/CuO |
| Adhesion rating | 0B | 2B | 3B | 4B |
Comparative example 1
The organic materials in the examples 1-3 are respectively replaced by PVDF or PTFE emulsion in equal quantity, and the prepared films can improve the heat release performance of the energetic materials, and through experimental researches, the film forming property of the 6 groups of films is poor, the adhesive force is not obviously improved, the special adhesive tape is stuck, the film is still seriously fallen, and the adhesive force reaches 1 grade at most. The main reason is that PVDF or PTFE has poor film forming property and poor effect of improving the adhesive force of the electrophoretic deposition energetic film.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for improving the adhesion of an electrophoretically deposited energetic film, comprising: the method comprises the following steps:
(1) Adding Al or metal oxide into an organic solvent according to the mass ratio of 1:2, and performing ultrasonic dispersion to obtain a suspension, wherein the metal oxide is CuO, and the organic solvent is isopropanol, acetone, methanol, ethanol and acetylacetone;
(2) Adding an organic material into the mixed solution, and performing ultrasonic treatment to obtain a solution, wherein the organic material is tridecafluorooctyl triethoxysilane;
(3) The suspension in the step (1) is used as an electrophoretic deposition solution, a cathode and an anode are placed, and after the power is on, a film is deposited on the surface of the cathode;
(4) Immersing the film in the step (3) into the solution in the step (2), standing for 5-30s, and then drying in vacuum.
2. The method for improving the adhesion of an electrophoretically deposited energetic film of claim 1, wherein: the weight fraction of Al and metal oxide in the organic solvent in the step (1) is 0.1-0.5%.
3. The method for improving the adhesion of an electrophoretically deposited energetic film of claim 1, wherein: the mixed solution in the step (2) is deionized water and absolute ethyl alcohol.
4. The method for improving the adhesion of an electrophoretically deposited energetic film of claim 3, wherein: dissolving tridecafluorooctyl triethoxysilane in the step (2) in absolute ethyl alcohol and deionized water to prepare a solution, wherein the concentration of the solution is between 0.1mol/L and 1.0mol/L, and uniformly mixing by ultrasonic treatment for 10-15 min.
5. The method for improving the adhesion of an electrophoretically deposited energetic film of claim 1, wherein: the electrophoretic deposition voltage in the step (3) is 100-150V, and the deposition time is not less than 2min.
6. The method for improving the adhesion of an electrophoretically deposited energetic film of claim 1, wherein: and (3) the cathode and the anode in the step (3) are pure copper sheets, pure titanium sheets, nickel sheets, iron sheets or stainless steel sheets.
7. An energetic film produced by the method of any one of claims 1-6.
8. Use of an energetic film prepared by the method of any one of claims 1-6 in a micro-nano energetic device.
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