CN104988560B - A kind of Al/MoO3Preparation method of the nanometer thermite containing energy film - Google Patents
A kind of Al/MoO3Preparation method of the nanometer thermite containing energy film Download PDFInfo
- Publication number
- CN104988560B CN104988560B CN201510457857.0A CN201510457857A CN104988560B CN 104988560 B CN104988560 B CN 104988560B CN 201510457857 A CN201510457857 A CN 201510457857A CN 104988560 B CN104988560 B CN 104988560B
- Authority
- CN
- China
- Prior art keywords
- film
- nanometer
- moo
- containing energy
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
A kind of Al/MoO3Preparation method of the nanometer thermite containing energy film, the method is with nanometer aluminium powder and nano-sized molybdenum oxide powder as deposition agent, it is combined as additive using amino silicane coupling agent and polyethyleneimine (PEI), using electrophoretic deposition in suspension after electrophoretic deposition, dried obtains Al/MoO3Nanometer thermite film containing energy.The inventive method prepare membrane material film layer thickness, good adhesive force, the fine and close free from flaw of film layer, thermal discharge height, have good burning performance.
Description
Technical field
This patent disclosure relates generally to preparation method of the nanometer containing energy film, and in particular to Al/MoO3System of the nanometer containing energy membrane material
Preparation Method.
Background technology
Thermite is due to producing high temperature and release substantial amounts of heat during reaction, and the advantages of easily prepared, low toxicity, is commonly used for
Welding, projection property fragmentation, propellant etc..But the reaction power of thermite is discharged by mass transfer control between particle, its energy
Speed is slow, limits its application.Between the reactant of nanometer thermite, the area of unit mass atomic contacts is big, mass transfer and heat
The distance of conduction reduces, and reaction rate is greatly enhanced, therefore nanometer thermite is used as the representative in Nanocomposite Energetic Materials
Cause extensive concern.And in the nanometer thermite that at present prepared by report, Al/MoO3Thermite has that burning velocity is fast, heat release
Amount is big, therefore Al/MoO3Thermite has great application prospect.Al/MoO in recent years3Nanometer thermite is concentrated mainly on powder body
Preparation on, but the complicated process of preparation of powder body has the shortcomings that concordance is poor.Therefore by this with burning velocity advantage
Thermite Film Morphology, it will overcome the defect of powder body, it is more practical.
The method of the preparation nanometer thermite film of report has magnetron sputtering method, heat steaming-oxidation composite algorithm, heat to steam-electricity at present
Plating-oxidation composite algorithm and electrophoretic deposition etc..Wherein, electrophoretic deposition operation temperature is low, and equipment is simple, easy to operate, cost
It is low, easily deposit on complicated substrate.(Sullivan K T, Worsley MA, Kuntz the J D, et such as Sullivan, K.T.
Al.Combustion and Flame, 2012,159 (6), 2210-2218) Al/CuO has been prepared using electrophoretic deposition receive
(Zhang, the D. such as rice thermite film, Zhang, Daixiong；Li,X.；Qin,B.Materials Letters,2014,120,
Al/Fe is prepared using electrophoretic deposition 224-227)2O3Nanometer thermite film, but the deposition film and substrate of this method preparation
Poor adhesive force, easily there is crack, particle defect such as free settling in suspension.(ChangTong, LI Zhiyou, the MA such as normal open
Li,Zhou Kechao.Materials Science and Engineering ofPowder Metallurgy,2011,
(05), 760-767) Fe is improve using the method sintered after electrophoretic deposition2O3The compactness and adhesive force of film, but for preparation
Thermite film is not simultaneously applied to, because thermite easily occurs thermit reaction, dangerous high.
The content of the invention
It is an object of the invention to provide a kind of Al/MoO3Preparation method of the nanometer thermite containing energy film, solution adopt electrophoresis
When sedimentation prepares thermite film, deposition film is difficult to be obtained compared with thick film layers, poor with substrate adhesion, the problems such as particle free settling.
Al/MoO of the invention3Preparation method of the nanometer thermite containing energy film, the method are with nanometer aluminium powder and receive
Rice molybdenum trioxide powder is deposition agent, is combined as additive using amino silicane coupling agent and polyethyleneimine (PEI), using electrophoresis
In suspension after electrophoretic deposition, dried obtains Al/MoO to sedimentation3Nanometer thermite film containing energy.It is mentioned herein
Nanometer aluminium powder and nano-sized molybdenum oxide powder typically refer to powder body of the particle diameter in below 100nm.
In one particular embodiment of the present invention, comprise the steps：
(1) nanometer aluminium powder and nano-sized molybdenum oxide powder are added in disperse medium, are stirred, wherein total particle quality
Concentration is 5g/L～10g/L；Total particle quality refers to the gross mass of the nanometer aluminium powder of addition and nano-sized molybdenum oxide powder；
(2) first appropriate amino silicane coupling agent is added in disperse medium, after stirring, adds appropriate gathering
Aziridine, after stirring, forms suspension；
(3) insertion shifts to an earlier date two clean electrodes of pretreatment as substrate, carries out electrophoretic deposition；
(4) deposition film is dried.
Under preferable case, wherein 0.1wt.%～10wt.% of the addition of amino silicane coupling agent for total particle quality,
5wt.%～15wt.% of the addition of polyethyleneimine for total particle quality.In the case of further preferably, wherein amino silane
3wt.%～5wt.% of the addition of coupling agent for total particle quality, the addition of polyethyleneimine is total particle quality
5wt.%～8wt.%, under the preferred concentration, inventors be surprised to learn that, electrodeposition efficiency is higher than under other concentration conditions
Go out more than 20%.
Under preferable case, one or more combination of the disperse medium in water, ethanol, isopropanol and ethylene glycol.
Under preferable case, wherein described two electrodes are respectively selected from copper sheet, stainless steel substrates, titanium sheet, nickel sheet or conductive glass
Glass.
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.
Al/MoO of the invention3Preparation method of the nanometer thermite containing energy film, compare other preparation methoies, its
Advantage and good effect：(1) additive used in the present invention is amino silicane coupling agent and PEI mixed liquors, and film layer can be obtained
Thickness adjustable extent is wide, the fine and close difficult for drop-off thermite film layer higher with substrate adhesion.Test result indicate that, with amino
Silane coupler is combined with polyethyleneimine and can change molybdenum trioxide surface charge polarity as additive, improves particle surface
The quantity of electric charge, up to 100 μm, adhesive force is determined by the code test of adhesive tape method testing coating adhesive force for the thicknesses of layers of acquisition
Reach 4B standards, the 85% of thermal discharge accessibility theory thermal discharge.The feature can improve the controllability and practical application of film；
(2) adopt the nanometer thermite film that the preparation method of the present invention is prepared more uniform, reactant contact more preferably, improves original
The utilization rate of material, and the method is simple to operate, and reaction condition is gentle, and preparation process is easily controllable, cycle is short, economic and practical,
Low production cost, is suitable for large-scale production；(3) present invention is adapted to the composite membrane for preparing various particles.
Description of the drawings
Fig. 1 is Al/MoO3Photo of the nanometer thermite containing energy film；
Fig. 2 is Al/MoO3SEM photograph of the nanometer thermite containing energy film；
Fig. 3 is Al/MoO3XRD spectrum of the nanometer thermite containing energy film；
Fig. 4 is Al/MoO3DSC curve of the nanometer thermite containing energy film；
Fig. 5 is Al/MoO3Burning photo of the nanometer thermite containing energy film.
Specific embodiment
Accompanying drawing is combined below by specific embodiment to be described in detail the present invention.
Embodiment 1：
The ethanol that the nano-sized molybdenum oxide particle of the nano-aluminium particle and 0.75g of precise 0.25g is added to 100mL is molten
In liquid, ultrasound 30 minutes under the conditions of 25 DEG C, first by 0.03g γ aminopropyltriethoxy silanes (KH550) plus as arrived ethanol
In solution, ultrasound 10 minutes adds 0.05g PEI and forms suspension, and ultrasound 20 minutes, at once insertion two are processed clean
Nickel sheet electrode (5 × 2cm), be electrophoretic deposition 25 minutes under 250V in applied voltage, obtain deposition film, it is true at 80～150 DEG C
Empty drying baker is dried 5～12 hours, after cooling, that is, obtains Al/MoO3Nanometer thermite film containing energy.
With zeta potential instrument, field emission scanning electron microscope (SEM), X-ray energy dispersion spectrum (EDS), X-ray powder diffraction
(XRD), code test (ASTM D 3359-2009) of differential scanning calorimeter (DSC) and adhesive tape method testing coating adhesive force etc.
Structure and performance characterization are carried out to product.
As depicted in figs. 1 and 2, the Al/MoO for being prepared using the inventive method3Nanometer thermite film is smooth, fine and closely woven.
As shown in figure 3, product feature diffraction maximum and Al and MoO in standard JCPDS3Standard diagram card match, deposit
In the characteristic diffraction peak of both materials, and peak shape is good.
As shown in figure 4, the Al/MoO for obtaining3The DSC curve of nanometer thermite, its thermal discharge is theoretical thermal discharge
85%.
As shown in figure 5, the Al/MoO for obtaining3Nanometer thermite film combustibility is preferable.
The Al/MoO for obtaining3Nanometer thermite film measures adhesive force grade for 4B by ASTM D 3359-2009.
Comparative example 1：
It is similar to Example 1, γ aminopropyltriethoxy silane (KH550) is not except for the difference that added in disperse medium,
0.05g PEI are added only as additive.The Al/MoO for obtaining3Nanometer thermite film measures attachment by ASTM D 3359-2009
Power grade is 3B.
Embodiment 2：
The nano-sized molybdenum oxide particle of the nano-aluminium particle and 0.75g of precise 0.25g is added to the aqueous solution of 100mL
In, under the conditions of 25 DEG C, 0.05g γ aminopropyltriethoxy silanes (KH550) are first added to aqueous solution by ultrasound 30 minutes
In, ultrasound 10 minutes, the PEI for adding 0.1g form suspension, and ultrasound 20 minutes inserts two processed clean purples at once
Copper plate electrode (5 × 2cm), is electrophoretic deposition 25 minutes under 5V in applied voltage, obtains deposition film, dry in 100～150 DEG C of vacuum
Dry case is dried 5～12 hours, after cooling, that is, obtains Al/MoO3Nanometer thermite film containing energy.
The Al/MoO for obtaining3Nanometer thermite film measures adhesive force grade for 4B by ASTM D 3359-2009.
Comparative example 2：
It is similar to Example 2, γ aminopropyltriethoxy silane (KH550) is not except for the difference that added in disperse medium,
0.1g PEI are added only as additive.The Al/MoO for obtaining3Nanometer thermite film measures attachment by ASTM D 3359-2009
Power grade is 3B.
Embodiment 3：
The molybdenum trioxide particle of the nano-aluminium particle and 0.75g of precise 0.25g is added to the ethylene glycol and water of 100mL
(volume ratio is 1:1) in disperse medium, ultrasound 30 minutes under the conditions of 25 DEG C, then by 0.03g gamma-amino propyl triethoxies
Silane (KH550) is added in solution, ultrasound 10 minutes, is added 0.05g PEI and is formed suspension, and ultrasound was stood after 20 minutes
Two processed clean nickel sheet electrodes (5 × 2cm) of insertion are carved, is electrophoretic deposition 25 minutes under 250V in applied voltage, is obtained
Deposition film, is dried 5～12 hours in 200 DEG C of vacuum drying ovens, after cooling, that is, obtains Al/MoO3Nanometer thermite film containing energy.
The Al/MoO for obtaining3Nanometer thermite film measures adhesive force grade for 4B by ASTM D 3359-2009.
Comparative example 3：
It is similar to Example 3, γ aminopropyltriethoxy silane (KH550) is not except for the difference that added in disperse medium,
0.05g PEI are added only as additive.The Al/MoO for obtaining3Nanometer thermite film measures attachment by ASTM D 3359-2009
Power grade is 3B.
Embodiment 4：
The nano-sized molybdenum oxide particle of the nano-aluminium particle and 0.65g of precise 0.35g is added to the isopropanol of 100mL
In solution, ultrasound 30 minutes under the conditions of 25 DEG C, then Deca 0.1g γ-aminopropyltrimethoxysilane (KH540) is to solution
In, ultrasound 10 minutes adds 0.08g PEI and forms suspension, ultrasound insert after 20 minutes, at once two it is processed clean
Nickel sheet electrode (5 × 2cm), is electrophoretic deposition 25 minutes under 300V in applied voltage, obtains deposition film, in 75～150 DEG C of vacuum
Drying baker is dried 5～12 hours, after cooling, that is, obtains Al/MoO3Nanometer thermite film containing energy.
The Al/MoO for obtaining3Nanometer thermite film measures adhesive force grade for 4B by ASTM D 3359-2009.
Comparative example 4：
It is similar to Example 4, γ-aminopropyltrimethoxysilane (KH540) is not except for the difference that added in disperse medium, only
0.08g PEI are added as additive.The Al/MoO for obtaining3Nanometer thermite film measures adhesive force by ASTM D 3359-2009
Grade is 3B.
Embodiment 5：
The molybdenum trioxide particle of the nano-aluminium particle and 0.65g of precise 0.35g is added to the ethanol solution of 100mL
In, ultrasound 30 minutes under the conditions of 25 DEG C, then Deca 0.01g γ-aminopropyltrimethoxysilane (KH540) is to ethanol solution
In, ultrasound 10 minutes, then Deca 0.05g PEI forms suspension, ultrasound insert after 20 minutes, at once two it is processed clean
Titanium sheet electrode (5 × 2cm), is electrophoretic deposition 25 minutes under 300V in applied voltage, obtains deposition film, in 75～150 DEG C of vacuum
Drying baker is dried 5～12 hours, after cooling, that is, obtains Al/MoO3Nanometer thermite film containing energy.
The Al/MoO for obtaining3Nanometer thermite film measures adhesive force grade for 4B by ASTM D 3359-2009.
Comparative example 5：
It is similar to Example 5, γ-aminopropyltrimethoxysilane (KH540) is not except for the difference that added in disperse medium, only
0.05g PEI are added as additive.The Al/MoO for obtaining3Nanometer thermite film measures adhesive force by ASTM D 3359-2009
Grade is 3B.
By above example and comparative example it is found that using amino silicane coupling agent and polyethyleneimine combination as adding
Plus agent is more preferable as the adhesive force of the deposition film obtained by additive than alone polyethyleneimine, reaches 4B ratings above, and
And deposition film more even compact, thermal discharge is higher.
The Al/MoO prepared by the method for the present invention3Nanometer thermite membrane material containing energy has higher heat release due to which
Amount and burning velocity, can be widely used for the field of the initiating bridge film containing energy in priming system.
Claims (7)
1. a kind of Al/MoO3Preparation method of the nanometer thermite containing energy film, the method is with nanometer aluminium powder and nano-sized molybdenum oxide powder
For deposition agent, combined as disperse medium using one or more in water, ethanol, isopropanol and ethylene glycol, with amino silicone
Alkane coupling agent and polyethyleneimine (PEI) combination after electrophoretic deposition, are done using electrophoretic deposition in suspension as additive
Dry process obtains Al/MoO3Nanometer thermite film containing energy.
2. Al/MoO according to claim 13Preparation method of the nanometer thermite containing energy film, comprises the steps：
(1) nanometer aluminium powder and nano-sized molybdenum oxide powder are added in disperse medium, are stirred, wherein total particle mass concentration
For 5g/L～10g/L；
(2) first appropriate amino silicane coupling agent is added in disperse medium, after stirring, adds appropriate polyethylene
Imines, after stirring, forms suspension；
(3) insertion shifts to an earlier date two clean electrodes of pretreatment as substrate, carries out electrophoretic deposition；
(4) deposition film is dried.
3. Al/MoO according to claim 23Preparation method of the nanometer thermite containing energy film, wherein amino silicane coupling agent
Addition for total particle quality 0.1wt.%～10wt.%, the addition of polyethyleneimine is total particle quality
5wt.%～15wt.%.
4. Al/MoO according to claim 23Preparation method of the nanometer thermite containing energy film, wherein described two electrodes point
Xuan Zi not copper sheet, stainless steel substrates, titanium sheet, nickel sheet or electro-conductive glass.
5. Al/MoO according to claim 23Preparation method of the nanometer thermite containing energy film, the wherein drying in step (4)
Technique is vacuum drying.
6. Al/MoO according to claim 23Preparation method of the nanometer thermite containing energy film, wherein in step (1) and (2)
Stirring technique be ultrasonic disperse.
7. Al/MoO obtained in the preparation method described in a kind of one of employing claim 1-63Nanometer thermite film containing energy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510457857.0A CN104988560B (en) | 2015-07-29 | 2015-07-29 | A kind of Al/MoO3Preparation method of the nanometer thermite containing energy film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510457857.0A CN104988560B (en) | 2015-07-29 | 2015-07-29 | A kind of Al/MoO3Preparation method of the nanometer thermite containing energy film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104988560A CN104988560A (en) | 2015-10-21 |
| CN104988560B true CN104988560B (en) | 2017-03-29 |
Family
ID=54300446
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510457857.0A Expired - Fee Related CN104988560B (en) | 2015-07-29 | 2015-07-29 | A kind of Al/MoO3Preparation method of the nanometer thermite containing energy film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104988560B (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106319601B (en) * | 2016-10-13 | 2018-05-29 | 重庆大学 | A kind of preparation method of super-hydrophobic porous metal coating |
| CN106467977B (en) * | 2016-10-13 | 2018-08-14 | 重庆大学 | It is a kind of to prepare 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 |
| CN108517551B (en) * | 2018-04-10 | 2020-05-22 | 浙江工业大学 | Novel silicon-aluminum coating and preparation process thereof |
| 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 |
| CN109576765B (en) * | 2019-01-10 | 2020-11-06 | 重庆大学 | Nano Mg/Fe2O3Low-pressure preparation method of energetic film |
| CN109678631B (en) * | 2019-01-29 | 2020-12-22 | 中北大学 | Two-dimensional 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 |
| CN110308136B (en) * | 2019-06-25 | 2021-07-30 | 中国计量大学 | Preparation method and application of noble metal and MoO3 self-assembly material |
| CN111850655B (en) * | 2020-07-27 | 2023-02-28 | 重庆工商大学 | Method for preparing high-adhesion nano thermite coating by electrophoretic deposition and coating thereof |
| 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 |
| CN115417737B (en) * | 2022-09-28 | 2023-09-01 | 南京理工大学 | Molybdenum oxide-based thermite and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8231748B1 (en) * | 2011-08-18 | 2012-07-31 | The United States Of America As Represented By The Secretary Of The Navy | Scalable low-energy modified ball mill preparation of nanoenergetic composites |
-
2015
- 2015-07-29 CN CN201510457857.0A patent/CN104988560B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN104988560A (en) | 2015-10-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104988560B (en) | A kind of Al/MoO3Preparation method of the nanometer thermite containing energy film | |
| CN105017831B (en) | Water-based electric heating nano paint composition and coating and its preparation method and application | |
| WO2021093759A1 (en) | Preparation methods for modified graphene and slurry containing said modified graphene | |
| CN106467977B (en) | It is a kind of to prepare Al/Bi2O3The method of Energetic Nanomaterials laminated film | |
| CN103215630A (en) | Method for sealing aluminum alloy anode oxide film pore by adopting organic-inorganic composite silica sol | |
| CN105024076A (en) | Anode material for lithium-ion battery and preparation method and application of anode material | |
| JP6329966B2 (en) | Multi-stage method for coating steel before thermoforming | |
| TW201823154A (en) | Production of graphene | |
| CN108878145B (en) | Preparation method of dielectric material for high-energy-storage capacitor | |
| JP2020507550A (en) | Lithium mixed oxide particles coated with aluminum oxide and titanium dioxide and method for producing the same | |
| CN105228273A (en) | For the preparation of the precursor solution of semiconductor thermoelectric film, Electric radiant Heating Film and preparation method | |
| TW201503456A (en) | A ceramic electrolyte material comprising a modified polycrystalline lithium metal phosphate | |
| TW201016596A (en) | Method of manufacturing zinc oxide nanoparticles and zinc oxide nanoparticles | |
| CN108963338B (en) | Preparation method of electrolyte containing graphene | |
| TW202023713A (en) | Silver powder and manufacturing method thereof | |
| CN107293698A (en) | A kind of preparation method of tin ash/carbon negative pole material | |
| CN110483219B (en) | Cubic structure composite energetic material and preparation method thereof | |
| CN108950653A (en) | A kind of preparation method of graphene oxide-aluminium-molybdenum trioxide ternary nano composite energy-containing film | |
| CN107674577A (en) | A kind of CNT graphene inorganic zinc-rich anti-corrosive paint | |
| CN102685943B (en) | Nanometer material electrothermal film | |
| JP5105780B2 (en) | Seal material and solid oxide fuel cell using the seal material | |
| JP2018506493A (en) | Thin film wet deposition method | |
| CN109055933B (en) | Powder liquid phase plasma surface modification method and device thereof | |
| CN112751140B (en) | Diaphragm functional coating material for improving liquid retention capacity and safety performance of lithium ion battery electrolyte | |
| CN108862266B (en) | Preparation method of graphene oxide nano material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170329 Termination date: 20180729 |