CN108179456A - A kind of preparation method of nanometer of thermite film - Google Patents
A kind of preparation method of nanometer of thermite film Download PDFInfo
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- CN108179456A CN108179456A CN201711246538.0A CN201711246538A CN108179456A CN 108179456 A CN108179456 A CN 108179456A CN 201711246538 A CN201711246538 A CN 201711246538A CN 108179456 A CN108179456 A CN 108179456A
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- nanometer
- thermite
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- aluminium powder
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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
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
Abstract
The present invention relates to the preparation methods of a kind of nanometer of thermite film, belong to thermite technical field.The present invention is surface modified nano bismuth oxide by citric acid,Improve its stability in a solvent,Potassium nitrate is recrystallized to the surface for being precipitated and being coated on nanometer aluminium powder from solution again,The subsequent phase transformation of polyvinylpyrrolidone is precipitated and is coated on nanometer aluminium powder and the surface of potassium nitrate,And using electrophoretic deposition,By positively charged surface coating nano aluminium powder,Citric acid modification nano bismuth oxide discrete particles are deposited on copper-based bottom,Prepare a nanometer thermite film,Two kinds of particle distributions are more uniform,Soilless sticking phenomenon occurs,Nanometer thermite film is compared with powdery thermite,With preferable mechanical performance,It may be directly applied to miniature priming system device and micromass culture system,It is integrated with the device containing energy,Realize synthesis,Powder charge integration,The preparation process of the device containing energy can be simplified,And film-form is more closely knit,The energy or pressure output of the device containing energy can be improved.
Description
Technical field
The present invention relates to the preparation methods of a kind of nanometer of thermite film, belong to thermite technical field.
Background technology
Nanometer thermite is due to having many advantages, such as high reaction activity and high-energy density, it has also become Energetic Nanomaterials are studied
In an important directions, also increasingly arouse people's interest.Many researchers carry out in terms of the preparation of nanometer thermite
Extensive work, has expanded the application range of nanometer thermite.Nanometer thermite is as a kind of novel nano energetic material, property
Can advantage obtained tentative confirmation, be many for how this energetic material haveing excellent performance being committed in practical application
The target that researcher makes joint efforts.
Nanometer thermite is also known as super thermite, usually by nanometer aluminium powder and nano-metal-oxide or nonmetallic oxidation
The nano level metal base reaction system that object is obtained through combined processing.It is with energyreleaserate is fast, calorific value is high, igniting causes energy
Measure the advantages that low, less toxic, environmentally friendly.Another important feature of nanometer thermit reaction is to generate high temperature and high heat.By
There are the characteristics such as high-energy density and high-energy release rate in nanometer thermite, high request of the energetic material to energy can be met.
Therefore, hot spot for energetic material area research is had become for how to prepare the nanometer thermite haveing excellent performance.At present, nanometer
The each method processed of thermite mainly includes：Physical mixed, sol-gel method inhibit reaction ball milling method, independently fill method, physics gas
Phase sedimentation, atomic layer deposition etc..
Nanocomposite Energetic Materials are close for wishing that one side can give full play to high-energy in composite solidpropellant
The advantages of degree and high rate of release, propellant burning rate and energy can be improved.On the other hand, nano aluminum is composite solidpropellant
The good catalyst of main component ammonium perchlorate, by its it is compound after can not only improve dispersibility and catalytic effect, and can
It is acted on playing the concerted catalysis of the two, the excellent functional characteristic of nano-particle is made greatly to be improved, gives full play to it
As the effect of SOLID PROPELLANT COMBUSTION catalyst, but nanometer thermite particle is easily reunited, when nanometer thermite content compared with
Gao Shi, serious reunion influence reactivity worth.
Therefore, present invention research prepares the nanometer thermite that has excellent performance to obtain higher energy density.
Invention content
The technical problems to be solved by the invention：Easily reunite for nanometer thermite particle, when nanometer thermite content
When higher, the problem of serious reunion influences reactivity worth, provides the preparation method of a kind of nanometer of thermite film.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Nano bismuth oxide is taken to add in 20~30min of ultrasonic disperse in deionized water, add lemon acid for adjusting pH and is stirred anti-
2~3h is answered, obtains colloidal solution；
（2）It will be dried at 80~90 DEG C to constant weight after colloidal solution filtering washing, obtain citric acid modification nano bismuth oxide；
（3）Polyvinylpyrrolidone, potassium nitrate are taken, adds in deionized water and stirs evenly, add nanometer aluminium powder ultrasonic disperse
And be evaporated to dryness under reduced pressure, obtain surface coating nano aluminium powder；
（4）Surface coating nano aluminium powder, citric acid modification nano bismuth oxide are taken, 20~30min of ultrasonic disperse in acetone is added in, obtains
Electrophoresis liquid；
（5）Using the copper-based bottom of 2cm × 2cm as cathode, graphite flake is immersed in 10~15min of electrophoresis in electrophoresis liquid for anode, will be electric
Copper-based bottom after swimming is dried in vacuo 10~12h, obtains a nanometer thermite film.
Step（1）The adjusting pH is simultaneously stirred to react process to add in lemon acid for adjusting pH to 5~6, and it is heated to 70~
80 DEG C, 2~3h is stirred with 300~400r/min.
Step（3）The polyvinylpyrrolidone, potassium nitrate, nanometer aluminium powder parts by weight be 0.2~0.4 part of polyethylene pyrrole
Pyrrolidone, 5~10 parts of potassium nitrate, 2~4 parts of nanometer aluminium powders.
Step（4）The surface coating nano aluminium powder, citric acid modification nano bismuth oxide mass ratio be 1：0.8~1：
3.2。
Step（5）The electrophoretic parameters in order to control electrode spacing be 1.0~1.5cm, adjustings voltage be 40~60V, electrophoresis
10~15min.
Step（5）The process of vacuum drying is dry 10~12h under 0.85~0.95MPa at 30~40 DEG C.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is surface modified nano bismuth oxide by citric acid, improves its stability in a solvent, then by nitre
Sour potassium recrystallizes the surface for being precipitated and being coated on nanometer aluminium powder from solution, and the subsequent phase transformation of polyvinylpyrrolidone is precipitated and coats
On the surface of nanometer aluminium powder and potassium nitrate, and using electrophoretic deposition, using copper-based bottom as cathode, graphite flake is anode, by band just
Surface coating nano aluminium powder, the citric acid modification nano bismuth oxide discrete particles of electricity are deposited on copper-based bottom, prepare nano aluminum
Thermit powder film, thermite film surface occurs without apparent crack, bumps, relatively flat closely knit, and two kinds of particle distributions are more
Uniformly, soilless sticking phenomenon occurs；
（2）The present invention is using the potassium nitrate with the advantages that fusing point is low, relative molecular mass is small, and releasing oxygen is more, and decomposition heat is small
Good with corrosion resistance as oxidant, oxygen content is high, has the higher combustion heat, does not generate the poly- second of toxic and harmful gas
Alkene pyrrolidone is binding agent, improves nanometer thermite film energy, residue rate and ignition ability；
（3）Nanometer thermite film prepared by the present invention has preferable mechanical performance, can directly answer compared with powdery thermite
It for miniature priming system device and micromass culture system, is integrated with the device containing energy, realizes synthesis, powder charge integration, can simplify containing energy
The preparation process of device, and film-form is more closely knit, can improve the energy or pressure output of the device containing energy.
Specific embodiment
It takes 20~30g nano bismuth oxides, adds in 100~200mL deionized waters, with 300W 20~30min of ultrasonic disperse,
Lemon acid for adjusting pH is added to 5~6, and is heated to 70~80 DEG C, 2~3h is stirred with 300~400r/min, it is molten to obtain colloid
Colloidal solution is filtered to obtain filter residue by liquid, filter residue is washed with deionized 2~3 times, then filter residue is placed in drying box, 80~
It is dried at 90 DEG C to constant weight, obtains citric acid modification nano bismuth oxide, take 0.2~0.4g polyvinylpyrrolidones, 5~10g nitric acid
Potassium is added in 400~800mL deionized waters, is stirred 20~30min with 300~400r/min, is added 2~4g nanometer aluminium powders,
It with 20~30min of 300W ultrasonic disperses and is evaporated to dryness under reduced pressure, obtains surface coating nano aluminium powder, 5~10g surfaces is taken to coat nanometer
Aluminium powder, 8~16g citric acid modification nano bismuth oxides are added in 400~800mL acetone, with 300W 20~30min of ultrasonic disperse,
Electrophoresis liquid is obtained, using the copper-based bottom of 2cm × 2cm as cathode, graphite flake is immersed in for anode in electrophoresis liquid, and coordination electrode spacing is
1.0~1.5cm, adjusting voltage are 40~60V, 10~15min of electrophoresis, and the copper-based bottom after electrophoresis is put into vacuum drying oven,
30~40 DEG C, dry 10~12h, obtains a nanometer thermite film under 0.85~0.95MPa.
Example 1
20g nano bismuth oxides are taken, are added in 100mL deionized waters, with 300W ultrasonic disperse 20min, add citric acid adjusting
PH is heated to 70 DEG C to 5, stirs 2h with 300r/min, obtains colloidal solution, colloidal solution is filtered to obtain filter residue, uses deionization
Water washing filter residue 2 times, then filter residue is placed in drying box, it is dried at 80 DEG C to constant weight, obtains citric acid modification nano bismuth oxide,
0.2g polyvinylpyrrolidones are taken, 5g potassium nitrate is added in 400mL deionized waters, is stirred 20min with 300r/min, is added
2g nanometer aluminium powders with 300W ultrasonic disperses 20min and are evaporated to dryness under reduced pressure, and obtain surface coating nano aluminium powder, and 5g surfaces is taken to coat
Nanometer aluminium powder, 8g citric acid modification nano bismuth oxides add in 400mL acetone, with 300W ultrasonic disperse 20min, obtain electrophoresis liquid,
Using the copper-based bottom of 2cm × 2cm as cathode, graphite flake is immersed in for anode in electrophoresis liquid, and coordination electrode spacing is 1.0cm, is adjusted
Voltage is 40V, electrophoresis 10min, and the copper-based bottom after electrophoresis is put into vacuum drying oven, and at 30 DEG C, dry 10h, obtains under 0.85MPa
Nanometer thermite film.
Example 2
25g nano bismuth oxides are taken, are added in 150mL deionized waters, with 300W ultrasonic disperse 25min, add citric acid adjusting
PH is heated to 75 DEG C to 5, stirs 2h with 350r/min, obtains colloidal solution, colloidal solution is filtered to obtain filter residue, uses deionization
Water washing filter residue 2 times, then filter residue is placed in drying box, it is dried at 85 DEG C to constant weight, obtains citric acid modification nano bismuth oxide,
0.3g polyvinylpyrrolidones are taken, 8g potassium nitrate is added in 600mL deionized waters, is stirred 25min with 350r/min, is added
3g nanometer aluminium powders with 300W ultrasonic disperses 25min and are evaporated to dryness under reduced pressure, and obtain surface coating nano aluminium powder, and 8g surfaces is taken to coat
Nanometer aluminium powder, 12g citric acid modification nano bismuth oxides add in 600mL acetone, with 300W ultrasonic disperse 25min, obtain electrophoresis
Liquid, using the copper-based bottom of 2cm × 2cm as cathode, graphite flake is immersed in for anode in electrophoresis liquid, and coordination electrode spacing is 1.5cm, is adjusted
Section voltage is 60V, electrophoresis 15min, and the copper-based bottom after electrophoresis is put into vacuum drying oven, at 40 DEG C, dry 12h under 0.95MPa,
Obtain nanometer thermite film.
Example 3
30g nano bismuth oxides are taken, are added in 200mL deionized waters, with 300W ultrasonic disperse 30min, add citric acid adjusting
PH is heated to 80 DEG C to 6, stirs 3h with 400r/min, obtains colloidal solution, colloidal solution is filtered to obtain filter residue, uses deionization
Water washing filter residue 3 times, then filter residue is placed in drying box, it is dried at 90 DEG C to constant weight, obtains citric acid modification nano bismuth oxide,
0.4g polyvinylpyrrolidones are taken, 10g potassium nitrate is added in 800mL deionized waters, is stirred 30min with 400r/min, is added
4g nanometer aluminium powders with 300W ultrasonic disperses 30min and are evaporated to dryness under reduced pressure, and obtain surface coating nano aluminium powder, and 10g surfaces is taken to coat
Nanometer aluminium powder, 16g citric acid modification nano bismuth oxides add in 800mL acetone, with 300W ultrasonic disperse 30min, obtain electrophoresis
Liquid, using the copper-based bottom of 2cm × 2cm as cathode, graphite flake is immersed in for anode in electrophoresis liquid, and coordination electrode spacing is 1.5cm, is adjusted
Section voltage is 60V, electrophoresis 15min, and the copper-based bottom after electrophoresis is put into vacuum drying oven, at 40 DEG C, dry 12h under 0.95MPa,
Obtain nanometer thermite film.
Reference examples：The nanometer thermite film of Hubei mold materials Co., Ltd production.
The nanometer thermite film of example and reference examples is detected, specific detection is as follows：
Measuring mechanical property：The static Micromechanics tensile property of homemade micro-stretching measuring instrument testing film.Sample is cut
For long 2.5cm, the fillet sample of wide 0.55cm, and pass through the mean breadth of each sample of vernier caliper measurement.So as to calculate
Go out the average traversal area of each sample.Sample is fixed on epoxy resin on an axis of sample stage, when epoxy resin is completely solid
After change, compressed air is passed through into air bearing, it is 40psi to keep compressed air pressure.Then control software is opened, starts horse
It reaches, records data.
Combustibility is tested：The combustibility of film is tested under normal pressure ar gas environment.
Specific testing result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Tensile strength/MPa | 12.32 | 12.08 | 12.20 | 7.50 |
| Burn rate/cmS-1 | 9.6 | 9.5 | 9.4 | 6.6 |
As shown in Table 1, the nanometer thermite film that prepared by the present invention has excellent mechanical strength and combustibility.
Claims (6)
1. the preparation method of a kind of nanometer of thermite film, which is characterized in that the specific steps are：
（1）Nano bismuth oxide is taken to add in 20~30min of ultrasonic disperse in deionized water, add lemon acid for adjusting pH and is stirred anti-
2~3h is answered, obtains colloidal solution；
（2）It will be dried at 80~90 DEG C to constant weight after colloidal solution filtering washing, obtain citric acid modification nano bismuth oxide；
（3）Polyvinylpyrrolidone, potassium nitrate are taken, adds in deionized water and stirs evenly, add nanometer aluminium powder ultrasonic disperse
And be evaporated to dryness under reduced pressure, obtain surface coating nano aluminium powder；
（4）Surface coating nano aluminium powder, citric acid modification nano bismuth oxide are taken, 20~30min of ultrasonic disperse in acetone is added in, obtains
Electrophoresis liquid；
（5）Using the copper-based bottom of 2cm × 2cm as cathode, graphite flake is immersed in 10~15min of electrophoresis in electrophoresis liquid for anode, will be electric
Copper-based bottom after swimming is dried in vacuo 10~12h, obtains a nanometer thermite film.
2. the preparation method of a kind of nanometer of thermite film as described in claim 1, which is characterized in that step（1）The tune
Section pH is simultaneously stirred to react process to add in lemon acid for adjusting pH to 5~6, and be heated to 70~80 DEG C, is stirred with 300~400r/min
Mix 2~3h.
3. the preparation method of a kind of nanometer of thermite film as described in claim 1, which is characterized in that step（3）It is described poly-
Vinylpyrrolidone, potassium nitrate, nanometer aluminium powder parts by weight for 0.2~0.4 part of polyvinylpyrrolidone, 5~10 parts of potassium nitrate,
2~4 parts of nanometer aluminium powders.
4. the preparation method of a kind of nanometer of thermite film as described in claim 1, which is characterized in that step（4）The table
Bread covers nanometer aluminium powder, the mass ratio of citric acid modification nano bismuth oxide is 1：0.8~1：3.2.
5. the preparation method of a kind of nanometer of thermite film as described in claim 1, which is characterized in that step（5）The electricity
Electrode spacing is 1.0~1.5cm to parameter of swimming in order to control, and adjusting voltage is 40~60V, 10~15min of electrophoresis.
6. the preparation method of a kind of nanometer of thermite film as described in claim 1, which is characterized in that step（5）It is described true
Empty drying process is dry 10~12h under 0.85~0.95MPa at 30~40 DEG C.
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Cited By (4)
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| 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 |
| CN112899746A (en) * | 2021-02-05 | 2021-06-04 | 南京理工大学 | Method for reducing electrostatic sensitivity of cuprous azide film |
| CN114143962A (en) * | 2021-12-01 | 2022-03-04 | 重庆大学 | Al/CuO nano energetic product |
| CN116063135A (en) * | 2021-10-29 | 2023-05-05 | 南京理工大学 | High-activity composite aluminum powder capable of catalyzing ammonium perchlorate and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN112899746A (en) * | 2021-02-05 | 2021-06-04 | 南京理工大学 | Method for reducing electrostatic sensitivity of cuprous azide film |
| CN116063135A (en) * | 2021-10-29 | 2023-05-05 | 南京理工大学 | High-activity composite aluminum powder capable of catalyzing ammonium perchlorate and preparation method thereof |
| CN114143962A (en) * | 2021-12-01 | 2022-03-04 | 重庆大学 | Al/CuO nano energetic product |
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