CN109680309A - Super hydrophobic porous Al/CuO nanometers of aluminothermy composite material containing energy - Google Patents
Super hydrophobic porous Al/CuO nanometers of aluminothermy composite material containing energy Download PDFInfo
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- CN109680309A CN109680309A CN201910169677.0A CN201910169677A CN109680309A CN 109680309 A CN109680309 A CN 109680309A CN 201910169677 A CN201910169677 A CN 201910169677A CN 109680309 A CN109680309 A CN 109680309A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
Abstract
Super hydrophobic porous Al/CuO nanometers of aluminothermy composite material containing energy, preparation method is ingenious to combine hydrogen template, high-temperature oxidation and electrophoretic deposition: using first and Porous Cu is prepared by regulation depositing operation as template using bubble hydrogen and quickly obtains porous C uO in conjunction with high-temperature oxydation;Then it is followed successively by electrode basement and realizes that the Controllable assembly of nano-aluminium particle finally realizes the preparation of super hydrophobic porous Al/CuO film containing energy by electrophoretic deposition.The present invention realizes the preparation of porous labyrinth energetic material, and overcomes the deficiencies of preparation processes such as magnetron sputtering are at high cost, process conditions are harsh.The thin-film material thermal energy output of this method preparation is strong and heat release stability is good;In addition, the simple process that the present invention uses, film forming efficiency is high, and universality is good, and prospects for commercial application is good.
Description
Technical field
The present invention relates to a kind of preparation methods for preparing Energetic Nanomaterials laminated film, specifically, being related to a kind of super
Al/CuO nanometers of aluminothermy composite material containing energies of hydrophobic porous.
Background technique
Energetic material (Energetic Materials) is used as a kind of reactive explosive, broadly refers to certain external
Under trigger condition, fast chemical reaction can be independently carried out, and discharges a substance of big energy.The material containing energy studied at present
Material mainly includes propellant powder, propellant, thermite, explosive and pyrotechnic compound etc..Most of all, the exothermicity of aluminothermy material
It is different greatly that degree is showed under the size of different stage, the development of the thermite of traditional thermite, that is, micron level is still insufficient
To overcome reaction speed slow, the response delay time is long, and thermal discharge is small and the shortcomings that concentration.Therefore, in recent years, nanoscale aluminium
Thermit powder i.e. at least one group is divided into nanoscale one kind thermite, causes extensive concern and deep exploration.The study found that
The more other traditional energetic materials of the performance of nanometer thermite film have better controllability and validity.
So far, in order to effectively promote the performance of nanometer thermite, corresponding preparation method is also too numerous to enumerate.It is main
It to include physical mixed method, collosol and gel-aeroge method, physical vaporous deposition, self-assembly method and inhibition reaction ball milling method.
Such as X.L.Hu (X.L.Hu, X.Liao, L.Q.Xiao et al.Propellants, Explosives, Pyrotechnics,
Al/Fe 2015,40:867-872) et al. has been prepared by quick physical mixed method2O3Thermite, but the method is extremely difficult
Effectively film forming, and material distributing homogeneity is poor.In addition, Egan (G.C.Egan, E.J.Mily, J.-P.Maria et
Al.The Journal of Physical Chemistry C, 2015,119 (35): 20401-20408) et al. use magnetic control
Sputtering method is prepared for multilayer Al/CuO aluminothermy system, and dazzling white flame occurs in electricity consumption pulse firing.Although the method film
Multi-layers distributing is uniform, but technological operation difficulty is big, and at high cost, is unfavorable for industrial production.Therefore, type uniform for structure is received
The critical bottleneck for being still energetic material field of the low-cost high-efficiency preparation of rice thermite.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of super hydrophobic porous Al/CuO nanometers of aluminothermy composite material containing energy,
It can effectively overcome above-mentioned certain or certain disadvantages.
A kind of preparation method of Al/CuO nanometers of aluminothermy composite material containing energies according to the present invention, comprising:
Electrolyte is provided, wherein HNO3With Cu (NO3)2Molar concentration rate be 5:1 or so, chloride ion content is 100~
200mg/L, polyethylene glycol (PEG) content are 0.1~0.5g/L;
The electrochemical deposition of Cu is carried out on cathode using above-mentioned electrolyte, wherein cathode and anode spacing are 1.5cm left
The right side, current density are 1~4A2/cm;
(porous) CuO is obtained by high-temperature oxydation is carried out after (porous) Cu deposited on cathode cleaning, wherein high-temperature oxydation
Heating rate is 20 DEG C/min, and oxidizing temperature control is at 300~500 DEG C, oxidization time 2h;
By nanoscale aluminium powder in ultrasonic disperse under confined conditions by isopropanol, ethyl acetoacetate, Tween 80 (poly- sorb
Ester 80, C64H124O26) and dodecyl triethoxysilane composed by form suspension in mixed dispersion liquid, isopropanol,
The volume ratio of ethyl acetoacetate, Tween 80 and dodecyl triethoxysilane is 1:2:10-4: 10-4, the concentration model of aluminium powder
It encloses for 0.5~2.5g/L, the ultrasonic disperse time is 5~25min, and temperature is controlled in 298 ± 1K;
Using the cathode for being formed with CuO thereon as working electrode, keep spacing for 1.0cm with to electrode (anode), jointly
It is inserted perpendicularly into suspension and executes electrophoresis, so that Al/CuO nanometers of aluminothermy composite material containing energies are formed on cathode, wherein additional
Electric field is 4-24Vmm-1, temperature is 25 DEG C, 1~20min of sedimentation time.
It according to the method for the present invention, can also include: to turn Al/CuO nanometers of thermite composite material containing energies of gained rapidly
It moves to and dries 1h in vacuum oven under 373~393 ± 1K, then cool to room temperature.It later, can also be by the yin as substrate
Pole removing is removed in gained composite material.
According to the present invention, cathode can be formed by titanium sheet, copper sheet, stainless steel substrates or nickel sheet, preferably titanium sheet;Anode can also be with
It is similarly formed.
In the present invention, it is preferred to use PEG4000.
According to the second aspect of the invention, a kind of composite material is provided, is prepared by the above method.
The present invention prepares Porous Cu using the hydrogen of precipitation as template using high constant current first on cathode, then
One layer of porous copper oxide is obtained in cathode substrate by high-temperature oxydation, recycles the yin for being attached to one layer of porous copper oxide later
Novel super hydrophobic porous Al/CuO has been made containing can be thin directly as working electrode, by controllable electrophoretic deposition technique in pole substrate
Film or composite material.
Cathode substrate of the invention is further preferably further provided with geosutures, to form the suitable section of required size, from
And it is convenient for subsequent removing.In addition, as needed, can only remove (such as by simply breaking disconnected movement along geosutures execution)
Required amount of section, to facilitate the storage and carrying of remaining energetic material.
In short, the present invention at least has the advantages that
(1) super hydrophobic porous Al/CuO nanometers of aluminothermys composite material containing energy structure novel prepared by the present invention, distribution of particles
Uniformly, there is no agglomeration;
(2) aluminothermy material exothermic prepared by the present invention is rapid and detonation is functional;
(3) preparation process of the present invention is simple, low in cost;
(4) present invention realizes the contact of nanoscale between Al and CuO, avoids traditional thermite and is unevenly distributed and leads
The limited problem of the material internal mass transfer of cause;
(5) requirement to raw material and equipment is low, and simple operations, preparation cost is cheap, and rate of film build is fast, is suitble to industry raw
It produces;
(6) adhesive force is good for super hydrophobic porous Al/CuO nanometers of aluminothermy composite material containing energies of the invention and substrate, leads to
Crossing tape method test result part can reach 5B standard, accounts for and has great advantage in industrial production application.
Detailed description of the invention
Fig. 1 (a) and Fig. 1 (b) is the field of super hydrophobic porous Al/CuO nanometers of aluminothermy laminated films according to the present invention respectively
Emit scanning electron microscope FESEM figure;
Fig. 2 is the graph of pore diameter distribution of super hydrophobic porous Al/CuO nanometers of aluminothermy laminated films according to the present invention;
Fig. 3 is the water droplet Static Contact state of super hydrophobic porous Al/CuO nanometers of aluminothermy laminated films according to the present invention
Figure;
Fig. 4 is the exotherm figure of super hydrophobic porous Al/CuO nanometers of aluminothermy laminated films according to the present invention.
Specific embodiment
The present invention is further illustrated below by embodiment.It should be appreciated by those skilled in the art that following embodiment is
In order to better understand and realize the present invention, it is not intended to restrict the invention.
Embodiment 1
Electrode material is cut into 1 × 5cm2, and by 1 × 5cm2Effective area be exposed, by polishing, cleaning etc.
It is stand-by that processing is placed on vacuum oven.The mixing of accurate configuration 0.5mol/L nitric acid and 0.1mol/L copper nitrate solution is molten
Liquid 100mL, and it is slowly added to the copper chloride solution that concentration is 150mg/L, chloride ion is provided.In addition, a small amount of PEG4000 is added
(0.36g/L) is mixed afterwards and ultrasonic mixing 2h.Fixed electrode material carries out electrochemical deposition.Current density is 4A/cm2, deposition
Then 10min will carry out high-temperature oxydation and obtain porous C uO after obtained porous C u cleaning treatment.Wherein, the liter of high-temperature oxydation
Warm rate is 20 DEG C/min, and oxidizing temperature control is at 400 DEG C, oxidization time 2h.Then, it is added to after nanoscale aluminium powder being weighed
100mL isopropanol, ethyl acetoacetate, Tween 80 and dodecyl triethoxysilane mixed dispersion liquid in, corresponding body
Product is than being 1:2:10-4: 10-4And the total concentration range of solid powder is 1.0g/L.Seal ultrasonic disperse 20min.Ultrasonic temperature
Degree control is in 298 ± 1K.Using the porous C uO being prepared as working electrode, the electrode material handled well is to electrode and electricity
Interpolar is away from for 1cm, and common vertical is inserted into finely dispersed suspension and carries out electrophoretic deposition, and 25 DEG C of temperature, extra electric field is selected as
10Vmm-1, sedimentation time control in 15min, finally obtain super hydrophobic porous Al/CuO nanometers of aluminothermy laminated film.
Using field emission scanning electron microscope (FESEM), electron diffraction instrument (XRD), differential scanning calorimeter (DSC) etc. is to compound
Film product carries out surface topography and performance study is analyzed and characterized.As shown in Fig. 1 (a) and 1 (b), prepared using the method for the present invention
Super hydrophobic porous Al/CuO nanometers of aluminothermy composite materials have even porous.It can analyze the pore-size distribution of sample in Fig. 2
Percentage.In addition, showing the high hydrophobic angle of sample in Fig. 3 (close to 170 °), it was demonstrated that its super-hydrophobicity.It is in Fig. 4 it can be seen that super
The thermal discharge of Al/CuO nanometers of aluminothermy composite materials of hydrophobic porous may be up to thermal discharge 4.7MJ Kg-1.In addition, what is obtained is super-hydrophobic
There is porous Al/CuO nanometers of aluminothermy laminated film adhesive force grade to be up to 5B.
Embodiment 2
The other the same as in Example 1, the difference is that PEG4000 is not added in electrolyte, the copper film that experiment discovery is prepared
Porosity is unobvious, and then leads to the insufficient contact of last nano aluminum and copper oxide, and it is only real for obtaining thermal discharge by analysis
The 20% of sample in example 1, hydrophobic performance are weaker.In addition, adhesive force is slightly impacted, grade 4B.
Embodiment 3
The other the same as in Example 1, the difference is that using PEG4000 instead PEG2000, experiment finds the more of the copper film being prepared
Permeability is more obvious, is evenly distributed, but aperture is slightly smaller, and then contact of the last nano aluminum with copper oxide is caused not filled more
Point, thermal discharge sharp fall is obtained by analysis, the 65% of sample about in example 1.But product at this time still has height
Up to 168 hydrophobic angle.In addition, adhesive force is equally by larger impact, grade will be for 3B.
Embodiment 4
The other the same as in Example 1, the difference is that selecting ethyl alcohol: acetylacetone,2,4-pentanedione: Tween 80 is dispersion liquid, and wherein volume ratio is 1:
2:10-5, discovery electrophoresis packaging efficiency is tested by taking deposition quality rate as an example, has dropped 11%, thermal discharge is slightly reduced, and can be neglected
Slightly.In addition, the phenomenon that slight crack and part reunion occurs in electrophoretic coating, there is larger impact in uniformity, and adhesive force also declines
Phenomenon is unfavorable for practical application.
As described above, the present invention is directed to same electrode basement, joint uses hydrogen template, high-temperature oxidation and controllable electric
The novel super hydrophobic porous Al/CuO that swimming deposition technique and being made is had excellent performance is containing can film.In addition, PEG4000, isopropanol,
The collaboration selection of ethyl acetoacetate and Tween 80 etc. is using uniformity height is further obtained, and energy density is high, and hydrophobicity is good
The strong product with broad prospect of application with adhesive force.
Claims (5)
1. a kind of preparation method of Al/CuO nanometers of aluminothermy composite material containing energy, comprising:
Electrolyte is provided, wherein HNO3With Cu (NO3)2Molar concentration rate be 5:1 or so, chloride ion content is 100~200mg/
L, PEG content are 0.1~0.5g/L;
The electrochemical deposition of Cu is carried out on cathode using above-mentioned electrolyte, wherein cathode and anode spacing are 1.5cm or so, electricity
Current density is 1~4A2/cm;
By the Cu deposited on cathode cleaning after carry out high-temperature oxydation obtain CuO, wherein the heating rate of high-temperature oxydation be 20 DEG C/
Min, oxidizing temperature control is at 300~500 DEG C, oxidization time 2h;
By nanoscale aluminium powder in ultrasonic disperse under confined conditions by isopropanol, ethyl acetoacetate, Tween 80 (polysorbate
80, C64H124O26) and dodecyl triethoxysilane composed by form suspension in mixed dispersion liquid, isopropanol, second
The volume ratio of ethyl acetoacetic acid ethyl ester, Tween 80 and dodecyl triethoxysilane is 1:2:10-4: 10-4, the total concentration model of aluminium powder
It encloses for 0.5g/L~2.5g/L, the ultrasonic disperse time is 5~25min, and temperature is controlled in 298 ± 1K;
Using the cathode for being formed with CuO thereon as working electrode, keep spacing for 1cm with to electrode, common vertical insertion suspends
Electrophoresis is executed in liquid, to form Al/CuO nanometers of aluminothermy composite material containing energies on cathode, wherein extra electric field is 4-
24Vmm-1, temperature is 25 DEG C, 1~20min of sedimentation time.
2. the method according to claim 1, further includes: be transferred quickly to Al/CuO nanometers of thermite composite material containing energies of gained
Dry 1h under 373~393 ± 1K, then cools to room temperature in vacuum oven.
3. method according to claim 2, further includes: by as the cathodic disbonding of substrate or removal in gained composite material.
4. according to the method in claim 3, wherein cathode is formed by titanium sheet, copper sheet, stainless steel substrates or nickel sheet.
5. the method according to claim 1, wherein the copper deposited on cleaning cathode includes: that the Cu that will be deposited on cathode is placed in ethyl alcohol
Be cleaned by ultrasonic 20min in distilled water at room temperature, be then transferred quickly in vacuum oven under 373~393 ± 1K dry 1h,
It is cooled to room temperature.
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Cited By (3)
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CN111362365A (en) * | 2020-01-17 | 2020-07-03 | 华中科技大学 | Unpowered nitrogen and phosphorus removal primary battery and preparation method and application thereof |
CN114143962A (en) * | 2021-12-01 | 2022-03-04 | 重庆大学 | Al/CuO nano energetic product |
CN114410147A (en) * | 2021-12-26 | 2022-04-29 | 南京理工大学 | Preparation method of nano thermite energetic printing ink |
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CN114410147A (en) * | 2021-12-26 | 2022-04-29 | 南京理工大学 | Preparation method of nano thermite energetic printing ink |
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