CN104371101B - Preparation method of carbon nano tube barium titanate polyaniline composite material - Google Patents
Preparation method of carbon nano tube barium titanate polyaniline composite material Download PDFInfo
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- CN104371101B CN104371101B CN201410634040.1A CN201410634040A CN104371101B CN 104371101 B CN104371101 B CN 104371101B CN 201410634040 A CN201410634040 A CN 201410634040A CN 104371101 B CN104371101 B CN 104371101B
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Abstract
The invention relates to the field of wave-absorbing materials and in particular relates to a preparation method of a carbon nano tube barium titanate polyaniline composite material. The preparation method of the carbon nano tube barium titanate polyaniline composite material comprises the step of coating the surface of a carbon nano tube barium titanate polyaniline composite material with polyaniline, and thus the carbon nano tube barium titanate polyaniline composite material is obtained. The carbon nano tube barium titanate polyaniline composite material has high dielectric property, an impedance matching frequency of the carbon nano tube barium titanate polyaniline composite material is adjustable and is adjusted, and conductivity is controlled by virtue of concentration of the added acid in a preparation process, so that a better wave-absorbing material with an adjustable impedance matching frequency is obtained.
Description
Technical field
The present invention relates to absorbing material field is and in particular to a kind of preparation of CNT barium titanate polyaniline composite material
Method.
Background technology
With developing rapidly of modern microwave electronic technology and modern radar, the impact to environment for the electromagenetic wave radiation increasingly increases
Greatly, after noise pollution, air pollution, water pollution, Contamination of Electromagnetic Wave has become the fourth-largest public affairs threatening human survival
Evil, has increasingly caused the attention of people to the protection of electromagnetic radiation.For the requirement of shelter of daily electromagnetic pollution, design and system
Standby absorbing material is the effective way solving electromagnetic pollution harm.Therefore the research of electromagnetic wave absorbent material is had extremely important
Meaning, the excellent absorbing material of processability becomes current study hotspot.
For a long time, human lives are in the environment of low electromagnetic level, but make rapid progress with scientific and technical, special
It is not electronics industry and the fast development of electronic product, the Highgrade integration of electronic devices and components, being highly miniaturized of electronic equipment,
Make the electromagnetic radiation of living environment increasingly serious, thus causing the electromagnetic pollution of environment.The dirt to environment for the common electromagnetic wave
Dye, is mainly manifested in following several respects: the harm that electromagnetic interference, electromagnetic wave leakage and electromagnetic radiation bring to health
Deng.Harm with electromagnetic radiation increasingly causes the concern of people, and the pollution how Electromagnetic Radiation on Environment being caused reduces
To minimum level, environmental protection, protection resident's is healthy, just becomes an important research topic.At present, electromagnetic protection
Major measure have two methods of electromagnetic wave shielding, electro-magnetic wave absorption.The former mainly in the form of reflection electromagnetic wave energy to electricity
Magnetic radiation is decayed；The latter is mainly decayed to electromagnetic radiation in the form of electromagnetic wave absorption energy.Electromagnetic shielding is general
It is using low-resistance metal good conductor or conductive resin material, when electromagnetic radiation is by these conductors of air directive, in metal
The surface of conductor will produce reflection and refraction effect, electromagnetic shielding be exactly using metallic conductor to the reflection effect of electromagnetic radiation with
Sink effect suppresses the purpose of electromagnetic radiation to reach.And electro-magnetic wave absorption is by absorbing material, electromagnetic wave to be absorbed.
Absorbing material is that one kind makes incident electromagnetic wave enter material internal to greatest extent, and being capable of effective attenuation by absorption incoming electromagnetic
Ripple, and its electromagnetic energy is converted into heat energy and dissipates or make a kind of functional material that electromagnetic wave disappears because of interference.
Various carbon-based materials, including carbon black, carbon nano-fiber, CNT and Graphene, because they have uniqueness
Structure, is gradually exploited in electromagnetic wave field, particularly CNT, and it has bigger reflectivity to electromagnetic wave, thus dropping
The low wavelength of electromagnetic wave, meanwhile, the large ratio of height to width of multi-walled carbon nano-tubes makes it possess very big interfacial area, and this is conducive to
Electron-transporting and electric conductivity, these all show that it possesses huge potential in absorbing material field.
And current, whether absorbing material macroscopic arts are applied to the microcosmic neck of absorbing material again with respect to CNT
Domain, all has blank.This limits the development of absorbing material from another point of view.
Content of the invention
In order to solve the problems referred to above that presently, there are, the present invention provides a kind of CNT barium titanate polyaniline composite material
Preparation method.Composite using the method preparation has excellent absorbing material, and this absorbing material has high dielectric property
Can, and its impedance matching frequency-adjustable adjusted.
In order to reach foregoing invention purpose, the present invention employs the following technical solutions:
A kind of preparation method of CNT barium titanate polyaniline composite material, comprises the following steps: take 30-50mg carbon to receive
Mitron barium titanate composite, distributes it to, in 20-30ml deionized water, add 20-25mg neopelex,
React 2h under ultrasound condition, obtain suspension；By the hydrochloric acid of 5mmol aniline monomer and the 0.5-5mol/l of 1-8ml, it is being stirred continuously
Under, gradually add to suspension system, obtain suspension system；The ammonium persulfate of 5mmol is dissolved into the deionized water of 10ml
In, obtain ammonium persulfate solution；Suspension system and ammonium persulfate solution are all cooled to -10-0 DEG C in advance, then that ammonium persulfate is molten
Drop adds in suspension system with the speed of 1-2ml/min, under ice bath react 5-24h, finally by products therefrom spend from
Sub- water and ethanol clean repeatedly to colourless, obtain CNT barium titanate polyaniline composite material.
Although CNT barium titanate composite has good absorbing property, it inhales wave frequency rate, in impedance matching
But deficiency is there is, by polyaniline being formed ternary heterojunction structure with CNT barium titanate composite and preparing on adjustable
After obtaining trielement composite material, thus realizing that electric conductivity is controlled, its way of realization is to be reached with adjusting the acid concentration of addition.
Preferably, described suspension system or dropping have in the suspension system of ammonium sulfate is additionally added 10-30mg diformazan
Base sulfoxide.
With the reduction of temperature, can carry out towards the reaction being conducive to suspension system and ammonium persulfate solution, but be as
The reduction of temperature, occurs icing phenomenon in reaction system, in order to ensure reaction can be smoothed out it is necessary to avoid freezing to anti-
The adverse effect answered, after adding dimethyl sulfoxide (DMSO), not only can make the freezing point of system reduce, dimethyl sulfoxide (DMSO) can simultaneously
Accelerate the reaction of ammonium sulfate, promote reaction to carry out to positive direction.
Preferably, described suspension system or dropping have the carboxylic being additionally added 10-20mg in the suspension system of ammonium sulfate
Methylcellulose.
In the present invention, unstable in the polyaniline of CNT barium titanate composite cladding and the bond strength of base material
Fixed, add carboxymethylcellulose calcium can improve the bond strength of polyaniline and base material, eliminate the place follow-up to the product of preparation
Science and engineering sequence, saves the process time.Thus not only optimizing preparation technology, and improve the stability of product.
Preferably, the preparation method of described CNT barium titanate composite comprises the following steps:
(1) CNT is added in red fuming nitric acid (RFNA), at 115 DEG C, stirring reaction 6 hours, red fuming nitric acid (RFNA) and CNT
Weight than for 50:1；After reaction terminates, cool down and filter, then cleaned CNT to neutrality using deionized water；
(2) preparation of metatitanic acid barium precursor
The barium acetate of 5mmol is dissolved in 5ml glacial acetic acid and the mixed solution of 20ml absolute ethyl alcohol, in 60 DEG C of water-bath
Middle stirring 30min, is dissolved with abundant, obtains solution a；
5mmol isopropyl titanate is dissolved in 10ml absolute ethyl alcohol and the mixed solution of 1ml deionized water, stirring
15min, makes fully to dissolve, and obtains solution b；
Mol ratio according to ba and ti is 1:1, b and a is measured, then the solution measuring b is added to solution a
In, after fully mixing, react 2-3h under 60 DEG C of water-baths, finally at room temperature after ageing more than 24h, obtain barium titanate forerunner
Body；
(3) preparation of CNT barium titanate composite
CNT 100mg after step (1) is processed is scattered in 40-60ml metatitanic acid barium precursor, ultrasonic disperse
It is suspension after 30min, then by suspension in 40 DEG C of water-baths, keep 4h under stirring condition, finally suspension is filtered, gained
Product, under argon gas atmosphere, is calcined 2-3h for 700 DEG C, is obtained CNT barium titanate composite.
Preferably, in described step (3), ultrasonic before be additionally added the disodium ethylene diamine tetraacetate of 50-80mg.
Due to polyaniline, after barium titanate surface is formed, bond strength is unstable, and disodium ethylene diamine tetraacetate can improve poly-
Aniline and the bond strength of barium titanate, thus the cladding thickness of polyaniline.
Compared with prior art, the fabric of method of the present invention preparation has the advantage that the present invention
1st, the CNT barium titanate polyaniline composite material of the present invention possesses more preferable absorbing property, its lighter weight,
Its suction wave frequency section is wider, absorptivity is good；
2nd, the composite of present invention preparation not only possesses high dielectric property, and its impedance matching frequency-adjustable obtains
Adjust；
3rd, the preparation method of the present invention, can be obtained more by reaching the control to electric conductivity to the concentration adding acid
The adjustable absorbing material of wave frequency rate, is inhaled in good impedance matching.
4th, the process step of the invention is simple, can directly be reacted to the carbon nanometer being coated with barium titanate by ammonium persulfate
Pipe is coated.
Specific embodiment
Below by specific embodiment, explanation is further described to technical scheme.
If no specified otherwise, the raw material employed in embodiments of the invention is raw material commonly used in the art, implements
Method employed in example, is the conventional method of this area.
The preparation method of the CNT barium titanate composite that the present invention adopts comprises the following steps:
(1) CNT is added in red fuming nitric acid (RFNA), at 115 DEG C, stirring reaction 6 hours, red fuming nitric acid (RFNA) and CNT
Weight than for 50:1；After reaction terminates, cool down and filter, then cleaned CNT to neutrality using deionized water；
(2) preparation of metatitanic acid barium precursor
The barium acetate of 5mmol is dissolved in 5ml glacial acetic acid and the mixed solution of 20ml absolute ethyl alcohol, in 60 DEG C of water-bath
Middle stirring 30min, is dissolved with abundant, obtains solution a；
5mmol isopropyl titanate is dissolved in 10ml absolute ethyl alcohol and the mixed solution of 1ml deionized water, stirring
15min, makes fully to dissolve, and obtains solution b；
Mol ratio according to ba and ti is 1:1, b and a is measured, then the solution measuring b is added to solution a
In, after fully mixing, react 2-3h under 60 DEG C of water-baths, finally at room temperature after ageing more than 24h, obtain barium titanate forerunner
Body；
(3) preparation of CNT barium titanate composite
CNT 100mg after step (1) is processed is scattered in 40-60ml metatitanic acid barium precursor, ultrasonic disperse
It is suspension after 30min, then by suspension in 40 DEG C of water-baths, keep 4h under stirring condition, finally suspension is filtered, gained
Product, under argon gas atmosphere, is calcined 2-3h for 700 DEG C, is obtained CNT barium titanate composite.
The preparation method of another kind of CNT barium titanate composite that the present invention adopts comprises the following steps:
Step (1) and (2) are same as described above, in step (3), are additionally added the ethylenediamine tetra-acetic acid of 50-80mg before ultrasonic
Disodium.
The CNT prepared using both approaches barium titanate composite is used for following embodiment.
Embodiment 1
A kind of preparation method of CNT barium titanate polyaniline composite material, comprises the following steps: take 30mg carbon nanometer
Pipe barium titanate composite, distributes it to, in 30ml deionized water, add 20mg neopelex, ultrasound condition
Lower reaction 2h, obtains suspension；By the hydrochloric acid of 5mmol aniline monomer and the 5mol/l of 1ml, under being stirred continuously, gradually add to
In suspension system, obtain suspension system；The ammonium persulfate of 5mmol is dissolved in the deionized water of 10ml, obtains persulfuric acid
Ammonium salt solution；Suspension system and ammonium persulfate solution are all cooled to 0 DEG C in advance, then ammonium persulfate solution are dripped the speed with 1ml/min
Degree adds in suspension system, reacts 24h under ice bath, finally repeatedly cleans products therefrom deionized water and ethanol to no
Color, obtains CNT barium titanate polyaniline composite material.
Embodiment 2
A kind of preparation method of CNT barium titanate polyaniline composite material, comprises the following steps: take 50mg carbon nanometer
Pipe barium titanate composite, distributes it to, in 20ml deionized water, add 25mg neopelex, ultrasound condition
Lower reaction 2h, obtains suspension；By the hydrochloric acid of 5mmol aniline monomer and the 0.5mol/l of 8ml, under being stirred continuously, gradually add
To suspension system, obtain suspension system；The ammonium persulfate of 5mmol is dissolved in the deionized water of 10ml, obtains over cure
Acid ammonium solution；Suspension system and ammonium persulfate solution are all cooled to -1 DEG C in advance, then drip ammonium persulfate solution with 2ml/min's
Speed adds in suspension system, under ice bath react 5h, finally by products therefrom deionized water and ethanol repeatedly clean to
Colourless, obtain CNT barium titanate polyaniline composite material.
Embodiment 3
A kind of preparation method of CNT barium titanate polyaniline composite material, comprises the following steps: take 30mg carbon nanometer
Pipe barium titanate composite, distributes it to, in 30ml deionized water, add 20mg neopelex, ultrasound condition
Lower reaction 2h, obtains suspension；By the hydrochloric acid of 5mmol aniline monomer and the 1mol/l of 5ml, 30mg dimethyl sulfoxide (DMSO), constantly stirring
Mix down, gradually add to suspension system, obtain suspension system；The ammonium persulfate of 5mmol is dissolved into the deionization of 10ml
In water, obtain ammonium persulfate solution；Suspension system and ammonium persulfate solution are all cooled to -5 DEG C in advance, then by ammonium persulfate solution
Dripping adds in suspension system with the speed of 1-2ml/min, reacts 10h, finally by products therefrom deionized water under ice bath
Repeatedly clean to colourless with ethanol, obtain CNT barium titanate polyaniline composite material.
Embodiment 4
A kind of preparation method of CNT barium titanate polyaniline composite material, comprises the following steps: take 40mg carbon nanometer
Pipe barium titanate composite, distributes it to, in 25ml deionized water, add 25mg neopelex, ultrasound condition
Lower reaction 2h, obtains suspension；By the hydrochloric acid of 5mmol aniline monomer and the 3mol/l of the 5ml of 5ml, 20mg dimethyl sulfoxide (DMSO), 10mg
Carboxymethylcellulose calcium, under being stirred continuously, gradually add to suspension system, obtain suspension system；Over cure by 5mmol
Sour ammonium is dissolved in the deionized water of 10ml, obtains ammonium persulfate solution；Suspension system and ammonium persulfate solution are all cooled in advance-
10 DEG C, then ammonium persulfate solution is dripped and add in suspension system with the speed of 1-2ml/min, react 24h under ice bath,
Afterwards products therefrom deionized water and ethanol are cleaned repeatedly to colourless, obtain CNT barium titanate polyaniline composite material.
Embodiment 5
A kind of preparation method of CNT barium titanate polyaniline composite material, comprises the following steps: take 30mg carbon nanometer
Pipe barium titanate composite, distributes it to, in 25ml deionized water, add 25mg neopelex, ultrasound condition
Lower reaction 2h, obtains suspension；By the hydrochloric acid of 5mmol aniline monomer and the 2mol/l of the 5ml of 5ml, 10mg dimethyl sulfoxide (DMSO), 20mg
Carboxymethylcellulose calcium, under being stirred continuously, gradually add to suspension system, obtain suspension system；Over cure by 5mmol
Sour ammonium is dissolved in the deionized water of 10ml, obtains ammonium persulfate solution；Suspension system and ammonium persulfate solution are all cooled in advance-
10 DEG C, then ammonium persulfate solution is dripped and add in suspension system with the speed of 1-2ml/min, react 8h under ice bath,
Afterwards products therefrom deionized water and ethanol are cleaned repeatedly to colourless, obtain CNT barium titanate polyaniline composite material.
Claims (2)
1. a kind of preparation method of CNT barium titanate polyaniline composite material is it is characterised in that comprise the following steps: takes
30-50mg CNT barium titanate composite, distributes it to, in 20-30ml deionized water, add 20-25mg dodecane
Base benzene sulfonic acid sodium salt, reacts 2h under ultrasound condition, obtains suspension；Salt by 5mmol aniline monomer and the 0.5-5mol/l of 1-8ml
Acid, under being stirred continuously, gradually adds to suspension system, obtains suspension system；The ammonium persulfate of 5mmol is dissolved into
In the deionized water of 10ml, obtain ammonium persulfate solution；Suspension system and ammonium persulfate solution are all cooled to -10-0 DEG C in advance, so
Dripping ammonium persulfate solution afterwards adds in suspension system with the speed of 1-2ml/min, reacts 5-24h under ice bath, finally will
Products therefrom deionized water and ethanol clean repeatedly to colourless, obtain CNT barium titanate polyaniline composite material, described
Suspension system or dropping have in the suspension system of ammonium persulfate solution and are additionally added 10-30mg dimethyl sulfoxide (DMSO), described suspension system
Or dropping has the carboxymethylcellulose calcium being additionally added 10-20mg in the suspension system of ammonium persulfate solution；
The preparation method of described CNT barium titanate composite comprises the following steps:
(1) CNT is added in red fuming nitric acid (RFNA), at 115 DEG C, stirring reaction 6 hours, the weight of red fuming nitric acid (RFNA) and CNT
Amount ratio is 50:1；After reaction terminates, cool down and filter, then cleaned CNT to neutrality using deionized water；
(2) preparation of metatitanic acid barium precursor
The barium acetate of 5mmol is dissolved in 5ml glacial acetic acid and the mixed solution of 20ml absolute ethyl alcohol, stirs in 60 DEG C of water-bath
Mix 30min, dissolved with abundant, obtain solution a；
5mmol isopropyl titanate is dissolved in 10ml absolute ethyl alcohol and the mixed solution of 1ml deionized water, stirs 15min, make
Fully dissolve, obtain solution b；
Mol ratio according to ba and ti is 1:1, b and a is measured, then the solution measuring b is added in solution a,
After fully mixing, react 2-3h under 60 DEG C of water-baths, finally at room temperature after ageing more than 24h, obtain metatitanic acid barium precursor；
(3) preparation of CNT barium titanate composite
CNT 100mg after step (1) is processed is scattered in 40-60ml metatitanic acid barium precursor, after ultrasonic disperse 30min
For suspension, then by suspension in 40 DEG C of water-baths, keep 4h under stirring condition, finally suspension filtered, products therefrom in
Under argon gas atmosphere, 700 DEG C of calcining 2-3h, obtain CNT barium titanate composite.
2. the preparation method of a kind of CNT barium titanate polyaniline composite material according to claim 1, its feature exists
In, in described step (3), ultrasonic before be additionally added the disodium ethylene diamine tetraacetate of 50-80mg.
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| CN105482111B (en) * | 2015-12-29 | 2017-12-15 | 陕西科技大学 | A kind of PANI/CoFe2O4/Ba0.4Sr0.6TiO3Absorbing material and preparation method |
| CN109096487A (en) * | 2017-06-20 | 2018-12-28 | 赵云飞 | Barium titanate/polyaniline composite material preparation method and applications |
| CN107835625B (en) * | 2017-09-18 | 2020-06-02 | 浙江理工大学 | Porous sheet cobalt/carbon composite wave-absorbing material and preparation method thereof |
| CN108774490B (en) * | 2018-05-31 | 2021-05-11 | 浙江理工大学 | Preparation method of microwave multi-band response multiple mesoporous structure wave absorber |
| CN110305318A (en) * | 2019-07-04 | 2019-10-08 | 大连交通大学 | A kind of polyaniline/barium titanate composite material and preparation method and application |
| CN114103348B (en) * | 2021-11-22 | 2023-03-14 | 四川大学 | Multilayer composite BOPE capacitor film and preparation method thereof |
| CN114957993A (en) * | 2022-06-02 | 2022-08-30 | 宁夏清研高分子新材料有限公司 | High-dielectric polyarylethersulfone material and preparation method thereof |
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| CN101475161B (en) * | 2009-01-13 | 2011-04-27 | 东华大学 | Method for preparing BaTiO3 / multi-wall carbon nano-tube (MWCNTs) nano composite material |
| CN103172972A (en) * | 2011-12-26 | 2013-06-26 | 深圳光启高等理工研究院 | Wave-absorbing material and preparation method thereof |
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