CN111850655A - Method for preparing high-adhesion nano thermite coating by electrophoretic deposition and coating prepared by method - Google Patents
Method for preparing high-adhesion nano thermite coating by electrophoretic deposition and coating prepared by method Download PDFInfo
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- CN111850655A CN111850655A CN202010732429.5A CN202010732429A CN111850655A CN 111850655 A CN111850655 A CN 111850655A CN 202010732429 A CN202010732429 A CN 202010732429A CN 111850655 A CN111850655 A CN 111850655A
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- 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
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- C01G49/00—Compounds of iron
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- C01G49/06—Ferric oxide (Fe2O3)
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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Abstract
The invention provides a method for preparing a high-adhesion nano thermite coating by electrophoretic deposition and a coating thereof, wherein an oil phase synthesis method, namely synthesizing octadecylamine and nitrate to prepare MOxNanoparticles, MOxMixing the nano particles with nano aluminum powder, dispersing the mixture in an organic solution, adding a dispersing agent to form a suspension, and obtaining a nano thermite Al-MO by an electrophoretic deposition methodxAnd (4) coating. The invention constructs the nano thermite Al-MO with good adhesive forcexThe coating solves the problem of Al-MO prepared by the current EPD methodxPoor adhesion of energetic coatings to substratesThe device is easy to fall off in a large area and fails due to the environment, and a universal strategy is provided for developing and rapidly preparing a practical initiating explosive device which is suitable for a complex storage and transportation environment and has high energy output. The nano-synthesis process has simple conditions and high coating assembling speed, is suitable for industrial production, can be widely applied to various fields such as national defense and military industry, micromotor systems and the like, and has good market application prospect.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a method for preparing a high-adhesion nano thermite coating by electrophoretic deposition and a coating prepared by the method.
Background
Thermite (Al-MO)x),Is prepared from Al and Metal Oxide (MO)xE.g. Fe2O3、CuO、Co3O4NiO, etc.) can be triggered by external energy to cause thermite reaction (2 xAl +3 MO)x=x Al2O3+3M + Q) releases a large amount of heat, and has unique and important application value in the national defense and military industry field due to the excellent heat release performance and deflagration performance. With the increasing demand for miniaturization and intelligence of weaponry in the 21 st century, the realization of the assembly of energetic materials in Micro-Electro-mechanical systems (MEMS) devices in the form of coatings is an urgent need for improving the energy output of igniters and thrusters. Al-MO compared to organic energetic materialsxThe higher triggering temperature leads the storage, transportation and use safety of the coating to be higher, and the assembly and preparation of the coating become the focus of attention of scholars at home and abroad.
Nano thermite (Al-MO)x) The coating has good adhesive force with the device substrate, is not easy to fall off in complex storage, transportation and use environments, and is one of the prerequisites that the energy-containing device can meet the practical application. Commonly used energetic material coating techniques include magnetron sputtering, electron beam sputtering, thermal evaporation, electrospinning, etc., which generally result in energetic coatings with good adhesion to device substrates, but also suffer from expensive equipment, complex operation, poor assembly adaptability to substrates of complex shape, etc.
In addition to the above method, the 2012 foreign scholars Sullivan first prepared nano Al/CuO coating by Electrophoretic deposition (EPD), and since EPD has the advantages of simple equipment, convenient method, low cost, and capability of adapting to substrates with complex and various shapes, it is used for preparing Al-MO-containing coatingxVarious strategies for energetic coatings have received attention from researchers. Of these, most exciting is that second-order (seconds or tens of seconds) preparation of the coating is expected to be achieved when the electrophoretic suspension nanoparticle concentration is significantly increased. Zhang successfully realizes Al/Fe2O3、Al/Co3O4EPD preparation of various energy-containing coatings such as Al/NiO, B/Ti and the like, and verification is carried out for the first timeEPD provides advantages and feasibility for rapid device-based assembly of energetic coatings on MEMS system micro-ignition bridges. Guo and Yin et al, achieve the preparation of energetic materials on substrates of different micro-morphologies, and disclose that the feasibility of EPD preparation of energetic coatings is not affected by the micro-morphology of the substrate.
However, due to the nano thermite (Al-MO)x) The contradiction between the thermite reaction triggering temperature and the sintering temperature of the coating (fig. 5) does not allow the use of post-sintering treatment to convert the nano thermite (Al-MO) into a nano thermitex) The microscopic morphology of the coating is transformed from a simple accumulation of nanoparticles to a continuous, solidified state. Therefore, the extremely poor adhesion between the energy-containing coating prepared by EPD and the device substrate leads to easy large-area cracking and shedding, and the key bottleneck which cannot be solved so far is still formed.
Disclosure of Invention
The invention aims to provide a method for preparing a high-adhesion nano thermite coating by electrophoretic deposition and a coating prepared by the method, which can effectively overcome some or all of the defects.
A method for preparing a high-adhesion nano thermite coating by electrophoretic deposition adopts an oil phase synthesis method to prepare metal oxide MOxNanoparticles, MOxMixing the nano particles with nano aluminum powder, dispersing the mixture in an organic solution, adding a dispersing agent to form a suspension, and obtaining the nano thermite coating by using an electrophoretic deposition method.
The method specifically comprises the following steps:
(1) heating octadecylamine to be molten, heating to 120-250 ℃, and adding MOxNitrate corresponding to nano particles is stirred at high temperature to prepare MOxCentrifugally collecting the nano particles for later use;
(2) polishing and washing the cathode and anode electrode plates, and then placing the cathode and anode electrode plates in a vacuum drying oven for drying for later use;
(3) mixing nano aluminum powder and MO obtained in step (1)xSequentially adding the nano particles into the dispersion liquid according to the weight ratio of 10: 1-1: 10, adding a proper amount of dispersing agent into the dispersion liquid, wherein the total concentration range of the solid powder is 1.0-20.0 g/L, and performing ultrasonic dispersion to form stable suspension;
(4) fixing the cathode and anode plates, inserting them verticallyElectrophoretic deposition is carried out in evenly dispersed suspension liquid, and the external electric field is 50-200Vcm-1After 5-30 minutes, obtaining a deposition film on the cathode plate;
(5) and drying the deposition film obtained by electrophoretic deposition.
The MOxM is one of Fe, Co, Ni, Cu and Zn.
In the step (1), the mass ratio of the octadecylamine to the nitrate is 40: 1-10: 1, the synthesis reaction temperature is 120-250 ℃, and the synthesis reaction time is 10-180 minutes.
In the step (3), the dispersion liquid is selected from isopropanol and ethanol, or a mixture of ethanol and acetylacetone according to a volume ratio of 1: 1; the dispersant is polyethyleneimine, nitric acid or hydrochloric acid.
The prepared nano thermite Al-MOxThe adhesion of the coating (above 4B) is significantly better than with commercially available MOxNano thermite Al-MO prepared from nano particlesxThe coating (2B) has uniform film surface distribution, good heat release performance and thermal stability.
The preparation method adopts an oil phase synthesis method, namely' octadecylamine (C1)8H37NH2ODA) -nitrate "synthesis, referred to herein as the ODA method, for the preparation of nano-MOsxMO preparedxThe coating and the substrate have extremely strong adhesion effect, and the reasons are that: octadecylamine is used as a solvent and a surfactant, and a long-chain oleophylic group of octadecylamine can be adsorbed on nano MO prepared from a nitrate metal precursorxSurface, long chain lipophilic group is expected to endow MOxStrong adhesion performance. In contrast, commercially available nanoparticles for EPD production of energetic coatings have been reported to have "clean" surfaces and no adhesion-forming elements. Therefore, the method utilizes the ODA oil phase synthesis method to prepare MOxNanoparticle replacement for commercially purchased MOxUsed as EPD powder raw material to prepare novel nano thermite Al-MOxCoating of MOxThe Al nano-particles and the MO are effectively improved by taking the Al nano-particles as a reactant in the energy-containing coating and simultaneously playing the role of a binderxIn order to construct a material with good adhesionThe energy-containing device provides a brand-new and effective technical scheme.
The invention constructs the nano thermite Al-MO with good adhesive forcexThe coating (M ═ Fe, Co, Ni and Cu) solves the problem of Al-MO prepared by the current EPD methodxThe problems of poor adhesion between the energetic coating and the substrate, easy large-area shedding and environmental failure are solved, and a universal strategy is provided for developing and rapidly preparing a practical initiating explosive device which is suitable for a complex storage and transportation environment and has high energy output. The method has simple nano synthesis process conditions and high coating assembling speed, is suitable for industrial production, can be widely applied to various fields such as national defense and military industry, micromotor systems and the like, and has good market application prospect.
Drawings
FIG. 1(a) is a schematic diagram showing comparative example 1 using commercially available Co3O4Al/Co by electrophoretic deposition3O4A nano-coating;
FIG. 1(b) shows the preparation of Co by ODA method in example 1 of the present invention3O4Al/Co by electrophoretic deposition3O4A nano-coating;
FIG. 2 shows Al/Co ratios of example 1 of the present invention3O4Characteristic XRD diffractogram of the nanocoating;
FIG. 3 shows Al/Co of example 1 of the present invention3O4The exotherm for the nanocoating;
FIG. 4 shows Al/Co photographed by the high-speed camera in embodiment 1 of the present invention3O4A burning picture of the nano-coating;
FIG. 5 is Al-MO prepared by prior art EPDxThe inherent contradiction between improving adhesion by coating sintering and triggering thermite reaction.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiment.
Example 1
Accurately weighing 20 g of octadecylamine, placing the octadecylamine in a round bottom flask, heating, melting and stirring the octadecylamine to 120 ℃, accurately weighing 2 g of cobalt nitrate, putting the cobalt nitrate into the octadecylamine, keeping the reaction temperature at 120 ℃, continuously stirring the cobalt nitrate for 10 minutes, stopping stirring, standing, cooling the cobalt nitrate to 80 ℃, pouring off the upper liquid ten minutesOctamine, collecting the bottom product of the flask, adding ethanol and cyclohexane at 10000 r.m.-1Centrifugally washing for three times to obtain nano Co3O4Particles.
0.03g of nano-aluminum particles and 0.07g of synthetic Co were weighed3O4Adding the nano particles into an ethanol solution, adding 1 mg of polyethyleneimine (1% of polyethyleneimine aqueous solution can be prepared according to the mass ratio), and carrying out ultrasonic treatment for 30 minutes under the condition of 298 +/-1K to form a stable suspension. Immediately, the pretreated cathode and anode materials of the titanium sheet are vertically inserted into the stable suspension liquid, and the external electric field is 200Vcm-1Electrophoretic deposition is carried out for 20 minutes, and the deposition temperature is controlled at 298 +/-1K. Then depositing the obtained Al/Co3O4And transferring the nano coating to a vacuum drying oven, drying for 1 hour at 333-373 +/-1K, and cooling to room temperature. Namely, Al/Co is obtained3O4And (4) nano coating.
The surface appearance and performance of the composite film product are researched, analyzed and characterized by a Zeta potentiometer, X-ray powder diffraction (XRD), a Field Emission Scanning Electron Microscope (FESEM), X-ray energy dispersion spectroscopy (EDX), a Differential Scanning Calorimeter (DSC), a high-speed camera and the like.
As shown in FIG. 1(b), Al/Co prepared by the method of the present invention3O4The nanocoating was smooth, evenly distributed, and had little agglomeration, relative to commercially available Co as shown in FIG. 1(a) of comparative example 1 below3O4Prepared Al/Co3O4The nano coating (a large amount of shedding occurs after the cutting by the knife) does not obviously shed after the cutting by the knife.
As shown in FIG. 2, Al/Co was prepared3O4Characteristic XRD diffraction peak of nano coating and Al and Co in standard JCPDS3O4The standard map cards are matched.
As shown in FIG. 3, Al/Co obtained3O4The nano coating has an exothermic curve with an exothermic amount up to 1890 J.g-1。
As shown in FIG. 4, Al/Co obtained3O4The combustion performance of the nano coating is good.
The obtained Al/Co3O4The nano coating adopts a standard test (ASTM D3359-2009) for testing the adhesion of the coating by a tape method to test the adhesion grade to be 4B.
Comparative example 1
Similar to example 1, except that Co was used in the electrophoretic deposition3O4Nanoparticles are commercially available. The adhesion rating was 2B using a standard tape method.
Example 2
Accurately weighing 20 g of octadecylamine, placing the octadecylamine in a round bottom flask, heating, melting and stirring to 180 ℃, accurately weighing 0.5 g of ferric nitrate, putting the ferric nitrate into the octadecylamine, keeping the reaction temperature at 180 ℃, continuing stirring for 30 minutes, stopping stirring, standing, cooling to 80 ℃, pouring out the upper liquid octadecylamine, collecting the bottom product of the flask, and using ethanol and cyclohexane at the rotation speed of 10000 r.m.min-1Centrifugally washing for three times to obtain the nano Fe2O3Particles.
0.04g of nano-aluminum particles and 0.06g of synthesized Fe were weighed2O3Adding the nano particles into an ethanol solution, adding 1 mg of polyethyleneimine (1% of polyethyleneimine aqueous solution can be prepared according to the mass ratio), and carrying out ultrasonic treatment for 30 minutes under the condition of 298 +/-1K to form a stable suspension. Immediately, the pretreated cathode and anode materials of the titanium sheet are vertically inserted into the stable suspension liquid, and the external electric field is 200Vcm-1Electrophoretic deposition is carried out for 20 minutes, and the deposition temperature is controlled at 298 +/-1K. Al/Fe obtained by the subsequent deposition2O3And transferring the nano coating to a vacuum drying oven, drying for 1 hour at 333-373 +/-1K, and cooling to room temperature. Thus obtaining Al/Fe2O3And (4) nano coating.
The Al/Fe obtained2O3The nano coating adopts a standard test (ASTM D3359-2009) for testing the adhesion of the coating by a tape method to test the adhesion grade to be 4B.
Comparative example 2
Similar to example 2, except that Fe was used in the electrophoretic deposition2O3Nanoparticles are commercially available. The adhesion rating was 2B using a standard tape method.
Example 3
Accurately weighing 20 g of octadecylamine, placing the octadecylamine in a round bottom flask, heating, melting and stirring the octadecylamine to 180 ℃, accurately weighing 2 g of nickel nitrate, putting the nickel nitrate into the octadecylamine, keeping the reaction temperature at 180 ℃, continuously stirring the nickel nitrate for 10 minutes, stopping stirring, standing, cooling the nickel nitrate to 80 ℃, pouring out the upper liquid octadecylamine, collecting a bottom product of the flask, and using ethanol and cyclohexane to rotate at the rotating speed of 10000 r.m.min-1And centrifuging and washing for three times to obtain the nano NiO particles.
Weighing 0.04g of nano aluminum particles and 0.06g of synthesized NiO nanoparticles, adding the nano aluminum particles and the synthesized NiO nanoparticles into an ethanol solution, adding 1 mg of polyethyleneimine (1% of polyethyleneimine aqueous solution can be prepared according to the mass ratio), and carrying out ultrasonic treatment for 30 minutes under the condition of 298 +/-1K to form a stable suspension. Immediately, the pretreated cathode and anode materials of the titanium sheet are vertically inserted into the stable suspension liquid, and the external electric field is 200Vcm-1Electrophoretic deposition is carried out for 20 minutes, and the deposition temperature is controlled at 298 +/-1K. And then transferring the Al/NiO nano coating obtained by the deposition to a vacuum drying oven, drying for 1 hour at 333-373 +/-1K, and cooling to room temperature. Thus obtaining the Al/NiO nano coating.
The obtained Al/NiO nano coating adopts a standard test (ASTM D3359-2009) for testing the adhesion of the coating by a tape method to test the adhesion grade to be 4B.
Comparative example 3
Similar to example 3, except that NiO nanoparticles used in electrophoretic deposition were commercially available. The adhesion rating was 2B using a standard tape method.
Example 4
Accurately weighing 20 g of octadecylamine, placing the octadecylamine in a round bottom flask, heating, melting and stirring the octadecylamine to 230 ℃, accurately weighing 0.5 g of copper nitrate, putting the copper nitrate into the octadecylamine, keeping the reaction temperature at 230 ℃, continuously stirring the mixture for 30 minutes, stopping stirring, standing, cooling the mixture to 80 ℃, pouring the upper liquid octadecylamine, collecting a bottom product of the flask, and using ethanol and cyclohexane at the rotation speed of 10000 r.min-1And centrifuging and washing for three times to obtain the nano CuO particles.
0.04g of nano-aluminum particles and 0.06g of synthesized CuO nanoparticles were weighed and added to the ethanol solution, and 1 mg of polyethyleneimine was addedAmine (1% of polyethyleneimine aqueous solution can be prepared according to the mass ratio) is subjected to ultrasonic treatment for 30 minutes under the condition of 298 +/-1K to form a stable suspension. Immediately, the pretreated cathode and anode materials of the titanium sheet are vertically inserted into the stable suspension liquid, and the external electric field is 200Vcm-1Electrophoretic deposition is carried out for 20 minutes, and the deposition temperature is controlled at 298 +/-1K. And then transferring the Al/CuO nano coating obtained by the deposition to a vacuum drying oven, drying for 1 hour at 333-373 +/-1K, and cooling to room temperature. Thus obtaining the Al/CuO nano coating.
The obtained Al/CuO nano coating adopts a standard test (ASTM D3359-2009) for testing the adhesion of the coating by a tape method to test the adhesion grade to be 4B.
Comparative example 4
Similar to example 4, except that CuO nanoparticles used in electrophoretic deposition were commercially available. The adhesion rating was 2B using a standard tape method.
Through comparison of a plurality of examples, the nano MO synthesized by using ODAxParticles instead of commercially purchased nano-MOsxParticles, Al-MO prepared by electrophoretic depositionxThe standard test of the adhesive force of the nano coating determines that the level reaches the standards of 4B and above 4B, and the nano coating has uniform surface distribution, good heat release performance and good thermal stability.
Claims (6)
1. The method for preparing the high-adhesion nano thermite coating by electrophoretic deposition is characterized in that an oil phase synthesis method is adopted to prepare metal oxide MOxNanoparticles, MOxMixing the nano particles with nano aluminum powder, dispersing the mixture in an organic solution, adding a dispersing agent to form a suspension, and obtaining the nano thermite coating by using an electrophoretic deposition method.
2. The method for preparing the high-adhesion nano thermite coating by electrophoretic deposition according to claim 1, comprising the following steps:
(1) heating octadecylamine to be molten, heating to 120-250 ℃, and adding MOxNitrate corresponding to nano particles is stirred at high temperature to prepare MOxCentrifugally collecting the nano particles for later use;
(2) polishing and washing the cathode and anode electrode plates, and then placing the cathode and anode electrode plates in a vacuum drying oven for drying for later use;
(3) mixing nano aluminum powder and MO obtained in step (1)xSequentially adding the nano particles into the dispersion liquid according to the weight ratio of 10: 1-1: 10, adding a proper amount of dispersing agent into the dispersion liquid, wherein the total concentration range of the solid powder is 1.0-20.0 g/L, and performing ultrasonic dispersion to form stable suspension;
(4) fixing cathode and anode plates, vertically inserting into uniformly dispersed suspension, performing electrophoretic deposition with an external electric field of 50-200Vcm-1After 5-30 minutes, obtaining a deposition film on the cathode plate;
(5) and drying the deposition film obtained by electrophoretic deposition.
3. The method of claim 1, wherein the MO is a high adhesion nano thermite coatingxM is one of Fe, Co, Ni, Cu and Zn.
4. The method for preparing the high-adhesion nano thermite coating by electrophoretic deposition according to claim 1, wherein the mass ratio of octadecylamine to nitrate in the step (1) is 40: 1-10: 1, the synthesis reaction temperature is 120-250 ℃, and the synthesis reaction time is 10-180 minutes.
5. The method for preparing the high-adhesion nano thermite coating by electrophoretic deposition according to claim 1, wherein the dispersion liquid in the step (3) is selected from isopropanol, ethanol, or a mixture of ethanol and acetylacetone according to a volume ratio of 1: 1; the dispersant is polyethyleneimine, nitric acid or hydrochloric acid.
6. Nano thermite coating obtained according to the preparation process of any one of claims 1 to 5.
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Cited By (2)
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CN113073373A (en) * | 2021-03-19 | 2021-07-06 | 重庆工商大学 | Electrophoretic deposition additive with wide applicability and deposition method |
CN113862755A (en) * | 2021-09-29 | 2021-12-31 | 巢湖学院 | Method for improving adhesion of electrophoretic deposition energetic film, improved energetic film and application |
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CN113862755B (en) * | 2021-09-29 | 2024-03-19 | 巢湖学院 | Method for improving adhesion of electrophoretic deposited energetic film, improved energetic film and application |
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