CN104988560A - Production method of Al/MoO3 nano-thermite energetic film - Google Patents
Production method of Al/MoO3 nano-thermite energetic film Download PDFInfo
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Abstract
A production method of a Al/MoO3 nano-thermite energetic film comprises the following steps: carrying out electrophoretic deposition in a suspension by adopting an electrophoretic deposition technology with nanometer aluminum powder and nanometer molybdenum trioxide powder as a deposition agent and an amino silane coupling agent and polyethylene imine (PEI) as an additive, and drying to obtain the Al/MoO3 nano-thermite energetic film. The film produced through the method has the advantages of thick film layer, good adhesion, compactness without cracks, high heat release and good combustion performance.
Description
Technical field
The present invention relates in general to the preparation method of nanometer containing energy film, is specifically related to Al/MoO
3nanometer is containing the preparation method of energy mould material.
Background technology
Thermite owing to producing high temperature during reaction and releasing a large amount of heat, and is easy to the advantages such as preparation, low toxicity, is commonly used for welding, projection property fragmentation, propelling agent etc.But the reaction power of thermite controls by mass transfer between particle, its energy release rate is slow, limits its application.Between the reactant of nano aluminum thermit powder, the area of unit mass atomic contacts is large, and mass transfer and heat conducting distance reduce, and speed of reaction greatly improves, and therefore nano aluminum thermit powder causes extensive concern as the representative in Nanocomposite Energetic Materials.And in the nano aluminum thermit powder of report preparation at present, Al/MoO
3thermite has that combustionvelocity is fast, thermal discharge is large, therefore Al/MoO
3thermite has great application prospect.Al/MoO in recent years
3nano aluminum thermit powder mainly concentrates in the preparation of powder, but the complicated process of preparation of powder, there is the shortcoming that consistence is poor.Therefore by this thermite Film Morphology with combustionvelocity advantage, the defect of powder will be overcome, more practical.
The method preparing nano aluminum thermit powder film of current report has magnetron sputtering method, heat steams-oxidation composite algorithm, heat steams-plating-oxidation composite algorithm and electrophoretic deposition etc.Wherein, electrophoretic deposition service temperature is low, and equipment is simple, and easy and simple to handle, cost is low, and the substrate of complexity easily deposits.Sullivan, K.T. (Sullivan K T is waited, Worsley MA, Kuntz J D, et al.Combustionand Flame, 2012,159 (6), 2210-2218) adopted electrophoretic deposition to prepare Al/CuO nano aluminum thermit powder film, Zhang, (Zhang, the D. such as Daixiong; Li, X.; Qin, B.Materials Letters, 2014,120,224-227) adopt electrophoretic deposition to prepare Al/Fe
2o
3nano aluminum thermit powder film, but the deposited film prepared of this method and substrate adhesion poor, easily there is crack, particle is the defect such as free settling in suspension.(ChangTong, LI Zhiyou, the MA Li such as normal open, Zhou Kechao.Materials Scienceand Engineering ofPowder Metallurgy, 2011, (05), 760-767) adopt electrophoretic deposition after the method that sinters improve Fe
2o
3the compactness of film and sticking power, but for preparing thermite film and inapplicable, because thermite easily thermite reaction occurs, dangerous high.
Summary of the invention
The object of this invention is to provide a kind of Al/MoO
3nano aluminum thermit powder is containing the preparation method of energy film, and when solution adopts electrophoretic deposition to prepare thermite film, deposited film is obtained comparatively thick film layers not easily, poor with substrate adhesion, the problems such as particle free settling.
According to Al/MoO of the present invention
3nano aluminum thermit powder is containing the preparation method of energy film, the method is for deposition agent with nanometer aluminium powder and nano-sized molybdenum oxide powder, using amino silicane coupling agent and polymine (PEI) coupling as additive, adopt electrophoretic deposition in suspension after electrophoretic deposition, drying treatment obtains Al/MoO
3nano aluminum thermit powder is containing energy film.Nanometer aluminium powder mentioned herein and nano-sized molybdenum oxide powder typically refer to the powder of particle diameter at below 100nm.
In one particular embodiment of the present invention, comprise the steps:
(1) join in dispersion medium by nanometer aluminium powder and nano-sized molybdenum oxide powder, stir, wherein total particle mass concentration is 5g/L ~ 10g/L; Total particle quality refers to the total mass of nanometer aluminium powder and the nano-sized molybdenum oxide powder added;
(2) first appropriate amino silicane coupling agent is joined in dispersion medium, after stirring, then add appropriate polymine, after stirring, form suspension;
(3) insert two clean electrodes of pre-treatment in advance as substrate, carry out electrophoretic deposition;
(4) deposited film is dry.
Under preferable case, wherein the add-on of amino silicane coupling agent is the 0.1wt.% ~ 10wt.% of total particle quality, and the add-on of polymine is the 5wt.% ~ 15wt.% of total particle quality.Under further preferable case, wherein the add-on of amino silicane coupling agent is the 3wt.% ~ 5wt.% of total particle quality, the add-on of polymine is the 5wt.% ~ 8wt.% of total particle quality, under this preferred concentration, contriver surprisingly finds, electrodeposition efficiency will exceed more than 20% than under other concentration conditions.
Under preferable case, described dispersion medium is selected from one or more combinations in water, ethanol, Virahol and ethylene glycol.
Under preferable case, wherein said two electrodes are selected from copper sheet, stainless steel substrates, titanium sheet, nickel sheet or conductive glass respectively.
Under preferable case, the drying process wherein in step (4) is vacuum-drying.
Under preferable case, the stirring technique wherein in step (1) and (2) is ultrasonic disperse.
According to Al/MoO of the present invention
3nano aluminum thermit powder is containing the preparation method of energy film, compare other preparation method, its advantage and positively effect: (1) additive used in the present invention is amino silicane coupling agent and PEI mixed solution, thicknesses of layers variable range can be obtained wide, the thermite rete of the fine and close difficult drop-off stronger with substrate adhesion.Experimental result shows, molybdic oxide surface charge polarity can be changed as additive using amino silicane coupling agent and polymine coupling, improve the quantity of electric charge of particle surface, the thicknesses of layers obtained can reach 100 μm, sticking power is measured by the standard test of adhesive tape method testing coating sticking power and reaches 4B standard, 85% of thermal discharge accessibility theory thermal discharge.This feature can improve controllability and the practical application of film; (2) the nano aluminum thermit powder film adopting preparation method of the present invention to prepare is more even, reactant contact is better, improve the utilization ratio of raw material, and the method is simple to operate, reaction conditions is gentle, and preparation process is easy to control, cycle is short, economic and practical, production cost is low, is suitable for scale operation; (3) the present invention is applicable to the composite membrane preparing multiple particle.
Accompanying drawing explanation
Fig. 1 is Al/MoO
3nano aluminum thermit powder is containing the photo of energy film;
Fig. 2 is Al/MoO
3nano aluminum thermit powder is containing the SEM photo of energy film;
Fig. 3 is Al/MoO
3nano aluminum thermit powder is containing the XRD figure spectrum of energy film;
Fig. 4 is Al/MoO
3nano aluminum thermit powder is containing the DSC curve of energy film;
Fig. 5 is Al/MoO
3nano aluminum thermit powder is containing the burning photo of energy film.
Embodiment
By reference to the accompanying drawings the present invention is described in detail below by specific embodiment.
Embodiment 1:
The nano-aluminium particle of precise 0.25g and the nano-sized molybdenum oxide particle of 0.75g join in the ethanolic soln of 100mL, under 25 DEG C of conditions ultrasonic 30 minutes, first 0.03g γ aminopropyltriethoxy silane (KH550) is added as in ethanolic soln, ultrasonic 10 minutes, add 0.05g PEI again and form suspension, ultrasonic 20 minutes, insert two processed clean nickel sheet electrodes (5 × 2cm) at once, electrophoretic deposition 25 minutes under impressed voltage is 250V, obtain deposited film, 80 ~ 150 DEG C of vacuum drying oven dryings 5 ~ 12 hours, after cooling, namely Al/MoO is obtained
3nano aluminum thermit powder is containing energy film.
With zeta potential instrument, field emission scanning electron microscope (SEM), X-ray energy dispersion spectrum (EDS), X-ray powder diffraction (XRD), the standard test (ASTM D 3359-2009) etc. of differential scanning calorimeter (DSC) and adhesive tape method testing coating sticking power carries out structure and performance characterization to product.
As depicted in figs. 1 and 2, the Al/MoO adopting the inventive method to prepare
3nano aluminum thermit powder film is smooth, fine and closely woven.
As shown in Figure 3, Al and MoO in product feature diffraction peak and standard JCPDS
3standard diagram card match, there is the characteristic diffraction peak of these two kinds of materials, and peak shape is good.
As shown in Figure 4, the Al/MoO obtained
3the DSC curve of nano aluminum thermit powder, its thermal discharge is 85% of theoretical thermal discharge.
As shown in Figure 5, the Al/MoO obtained
3nano aluminum thermit powder film combustionproperty is better.
The Al/MoO obtained
3it is 4B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Comparative example 1:
Similar to Example 1, unlike not adding γ aminopropyltriethoxy silane (KH550) in dispersion medium, only add 0.05g PEI as additive.The Al/MoO obtained
3it is 3B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Embodiment 2:
The nano-aluminium particle of precise 0.25g and the nano-sized molybdenum oxide particle of 0.75g join in the aqueous solution of 100mL, under 25 DEG C of conditions ultrasonic 30 minutes, first 0.05g γ aminopropyltriethoxy silane (KH550) is joined in the aqueous solution, ultrasonic 10 minutes, the PEI adding 0.1g again forms suspension, ultrasonic 20 minutes, insert two processed clean copper sheet electrodes (5 × 2cm) at once, electrophoretic deposition 25 minutes under impressed voltage is 5V, obtain deposited film, 100 ~ 150 DEG C of vacuum drying oven dryings 5 ~ 12 hours, after cooling, namely Al/MoO is obtained
3nano aluminum thermit powder is containing energy film.
The Al/MoO obtained
3it is 4B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Comparative example 2:
Similar to Example 2, unlike not adding γ aminopropyltriethoxy silane (KH550) in dispersion medium, only add 0.1g PEI as additive.The Al/MoO obtained
3it is 3B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Embodiment 3:
In the ethylene glycol that the nano-aluminium particle of precise 0.25g and the molybdic oxide particle of 0.75g join 100mL and water (volume ratio is 1:1) dispersion medium, under 25 DEG C of conditions ultrasonic 30 minutes, then 0.03g γ aminopropyltriethoxy silane (KH550) is joined in solution, ultrasonic 10 minutes, add 0.05g PEI again and form suspension, after ultrasonic 20 minutes, insert two processed clean nickel sheet electrodes (5 × 2cm) at once, electrophoretic deposition 25 minutes under impressed voltage is 250V, obtain deposited film, 200 DEG C of vacuum drying oven dryings 5 ~ 12 hours, after cooling, namely Al/MoO is obtained
3nano aluminum thermit powder is containing energy film.
The Al/MoO obtained
3it is 4B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Comparative example 3:
Similar to Example 3, unlike not adding γ aminopropyltriethoxy silane (KH550) in dispersion medium, only add 0.05g PEI as additive.The Al/MoO obtained
3it is 3B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Embodiment 4:
The nano-aluminium particle of precise 0.35g and the nano-sized molybdenum oxide particle of 0.65g join in the aqueous isopropanol of 100mL, under 25 DEG C of conditions ultrasonic 30 minutes, then 0.1g γ-aminopropyltrimethoxysilane (KH540) is dripped in solution, ultrasonic 10 minutes, add 0.08g PEI again and form suspension, after ultrasonic 20 minutes, insert two processed clean nickel sheet electrodes (5 × 2cm) at once, electrophoretic deposition 25 minutes under impressed voltage is 300V, obtain deposited film, 75 ~ 150 DEG C of vacuum drying oven dryings 5 ~ 12 hours, after cooling, namely Al/MoO is obtained
3nano aluminum thermit powder is containing energy film.
The Al/MoO obtained
3it is 4B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Comparative example 4:
Similar to Example 4, unlike not adding γ-aminopropyltrimethoxysilane (KH540) in dispersion medium, only add 0.08g PEI as additive.The Al/MoO obtained
3it is 3B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Embodiment 5:
The nano-aluminium particle of precise 0.35g and the molybdic oxide particle of 0.65g join in the ethanolic soln of 100mL, under 25 DEG C of conditions ultrasonic 30 minutes, then 0.01g γ-aminopropyltrimethoxysilane (KH540) is dripped in ethanolic soln, ultrasonic 10 minutes, drip 0.05g PEI again and form suspension, after ultrasonic 20 minutes, insert two processed clean titanium sheet electrodes (5 × 2cm) at once, electrophoretic deposition 25 minutes under impressed voltage is 300V, obtain deposited film, 75 ~ 150 DEG C of vacuum drying oven dryings 5 ~ 12 hours, after cooling, namely Al/MoO is obtained
3nano aluminum thermit powder is containing energy film.
The Al/MoO obtained
3it is 4B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Comparative example 5:
Similar to Example 5, unlike not adding γ-aminopropyltrimethoxysilane (KH540) in dispersion medium, only add 0.05g PEI as additive.The Al/MoO obtained
3it is 3B that nano aluminum thermit powder film records sticking power grade by ASTM D 3359-2009.
Can be found by above embodiment and comparative example, the sticking power of the deposited film obtained as additive as additive than alone polymine using amino silicane coupling agent and polymine coupling is better, all reach more than 4B grade, and deposited film even compact more, thermal discharge is higher.
By Al/MoO prepared by method of the present invention
3nano aluminum thermit powder containing higher thermal discharge and combustionvelocity can be had due to it by mould material, can be widely used in priming system containing can initiating bridge film field.
Claims (8)
1. an Al/MoO
3nano aluminum thermit powder is containing the preparation method of energy film, the method is for deposition agent with nanometer aluminium powder and nano-sized molybdenum oxide powder, using amino silicane coupling agent and polymine (PEI) coupling as additive, adopt electrophoretic deposition in suspension after electrophoretic deposition, drying treatment obtains Al/MoO
3nano aluminum thermit powder is containing energy film.
2. Al/MoO according to claim 1
3nano aluminum thermit powder, containing the preparation method of energy film, comprises the steps:
(1) join in dispersion medium by nanometer aluminium powder and nano-sized molybdenum oxide powder, stir, wherein total particle mass concentration is 5g/L ~ 10g/L;
(2) first appropriate amino silicane coupling agent is joined in dispersion medium, after stirring, then add appropriate polymine, after stirring, form suspension;
(3) insert two clean electrodes of pre-treatment in advance as substrate, carry out electrophoretic deposition;
(4) deposited film is dry.
3. Al/MoO according to claim 2
3nano aluminum thermit powder is containing the preparation method of energy film, and wherein the add-on of amino silicane coupling agent is the 0.1wt.% ~ 10wt.% of total particle quality, and the add-on of polymine is the 5wt.% ~ 15wt.% of total particle quality.
4. Al/MoO according to claim 2
3nano aluminum thermit powder is containing the preparation method of energy film, and described dispersion medium is selected from one or more combinations in water, ethanol, Virahol and ethylene glycol.
5. Al/MoO according to claim 2
3nano aluminum thermit powder is containing the preparation method of energy film, and wherein said two electrodes are selected from copper sheet, stainless steel substrates, titanium sheet, nickel sheet or conductive glass respectively.
6. Al/MoO according to claim 2
3nano aluminum thermit powder is containing the preparation method of energy film, and the drying process wherein in step (4) is vacuum-drying.
7. Al/MoO according to claim 2
3nano aluminum thermit powder is containing can the preparation method of film, and the stirring technique wherein in step (1) and (2) is ultrasonic disperse.
8. the Al/MoO adopting the described preparation method of one of claim 1-7 to obtain
3nano aluminum thermit powder is containing energy film.
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| CN105714357A (en) * | 2016-04-29 | 2016-06-29 | 中国工程物理研究院化工材料研究所 | Electrophoretic deposition charging method for energetic material |
| CN106319601A (en) * | 2016-10-13 | 2017-01-11 | 重庆大学 | Preparing method for super-hydrophobic type porous metal coating |
| CN106467977A (en) * | 2016-10-13 | 2017-03-01 | 重庆大学 | One kind prepares Al/Bi2O3The method of Energetic Nanomaterials laminated film |
| CN107245746A (en) * | 2017-04-28 | 2017-10-13 | 重庆大学 | Al/CuO thermites and preparation method thereof |
| CN108179456A (en) * | 2017-12-01 | 2018-06-19 | 姜向军 | A kind of preparation method of nanometer of thermite film |
| CN108517551A (en) * | 2018-04-10 | 2018-09-11 | 浙江工业大学 | A kind of System of Silica/Aluminum Microparticle coating and its preparation process |
| CN108950653A (en) * | 2018-06-06 | 2018-12-07 | 华电电力科学研究院有限公司 | A kind of preparation method of graphene oxide-aluminium-molybdenum trioxide ternary nano composite energy-containing film |
| CN109576765A (en) * | 2019-01-10 | 2019-04-05 | 重庆大学 | Nanometer Mg/Fe2O3The low pressure preparation method of the film containing energy |
| CN109678631A (en) * | 2019-01-29 | 2019-04-26 | 中北大学 | A kind of two dimension energetic material and preparation method thereof |
| CN109706508A (en) * | 2019-03-13 | 2019-05-03 | 重庆大学 | Hollow Mg/MnO2The preparation of super energetic material |
| CN110308136A (en) * | 2019-06-25 | 2019-10-08 | 中国计量大学 | A kind of noble metal and MoO3The preparation method and application of self-assembled material |
| CN111850655A (en) * | 2020-07-27 | 2020-10-30 | 重庆工商大学 | Method for preparing high-adhesion nano thermite coating by electrophoretic deposition and coating prepared by method |
| CN114032600A (en) * | 2021-11-12 | 2022-02-11 | 重庆大学 | Preparation method of Al/NiO energetic film based on electrophoretic deposition |
| CN114143962A (en) * | 2021-12-01 | 2022-03-04 | 重庆大学 | Al/CuO nano energetic product |
| CN115417737A (en) * | 2022-09-28 | 2022-12-02 | 南京理工大学 | Molybdenum oxide-based thermite and preparation method thereof |
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| CN105714357B (en) * | 2016-04-29 | 2017-10-24 | 中国工程物理研究院化工材料研究所 | Energetic material electrophoretic deposition loading method |
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| CN115417737B (en) * | 2022-09-28 | 2023-09-01 | 南京理工大学 | Molybdenum oxide-based thermite and preparation method thereof |
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