CN102977601B - Preparation method of manganese-zinc-ferrite-coated DBSA-modified carbon-nanotube-polyaniline composite wave-absorbing material - Google Patents
Preparation method of manganese-zinc-ferrite-coated DBSA-modified carbon-nanotube-polyaniline composite wave-absorbing material Download PDFInfo
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Abstract
The invention provides a preparation method of a manganese-zinc-ferrite-coated DBSA-modified carbon-nanotube-polyaniline composite wave-absorbing material. According to the invention, multi-wall carbon nanotube is modified by using dodecylbenzene sulfonic acid (DBSA); the modified carbon nanotube, MnSO4.H2O, Zn(NO3)2.6H2O, and Fe(NO3)3.9H2O are adopted as raw materials, and a manganese-zinc-ferrite-coated DBSA-modified carbon-nanotube composite material is prepared with a hydrothermal synthesis method; and the material is subjected to in-situ polymerization with aniline monomer, such that the manganese-zinc-ferrite-coated DBSA-modified carbon-nanotube-polyaniline composite wave-absorbing material is prepared. The composite material overcomes defects such as high density and poor dielectric loss of previous wave-absorbing materials, and has excellent impedance matching and loss characteristics. The material has important application value in the field of microwave absorption.
Description
Technical field
The invention belongs to electromagnetic wave absorbent material preparation field, the preparation method of the carbon naotube-polyaniline composite wave-suction material of the particularly coated DBSA modification of a kind of Mn-Zn ferrite.
Background technology
The nonmetal composite oxides with spinel structure that Mn-Zn ferrite is made up of manganese, zinc, iron, it is a kind of very important basic function material in the national economic development, compared with metallicl magnetic material of the same type, there is the physical and chemical performances such as high magnetic permeability, high resistivity, high saturation and magnetic intensity, low-coercivity and low-loss in high frequency, be widely used in electronics and information industry, electrical appliance industry, network of communication and the industry such as terminal and instrument.
Carbon nanotube had both had the intrinsic person's character of carbon materials, had again conduction and the thermal conductivity of metallic substance, heat-resisting, the erosion resistance of stupalith, the stitchability of textile fibres, and the lightweight of macromolecular material, workability.Carbon nanotube, as composite material reinforcement body, can make composite material exhibits go out good intensity, elasticity, fatigue resistance and isotropy, and therefore Carbon Nanotubes Reinforced Composites may bring the once leap of composite property.
Polyaniline is cheap with monomer whose, synthesis technique is simple, mechanism of doping effect is special, conductivity is excellent, stable good and special optical, electrical, magnetic property and getting more and more people's extensive concerning, and is considered to the most promising a kind of conducting polymer.To its synthesis, structure, characteristic and application, oneself has done a large amount of work to people, and achieves a series of important achievement, is widely used in many fields.Nowadays, the research of people's p-poly-phenyl amine is no longer confined to electricity field, finds, by after polyaniline and magneticsubstance compound, to show special optics, magnetics and electric property.
Therefore, take polyaniline conductive polymer as the coated DBSA modified carbon nano-tube-polyaniline composite material of Mn-Zn ferrite that matrix composition goes out, there is the dual nature of magnetic and electroconductibility, be integrate the advanced composite material that ferrite inhales ripple, carbon nanotube inhales ripple, conducting polymer inhales ripple, have broad application prospects in sensing technology, electromagnetic shielding and radar absorption etc.
Summary of the invention
The object of this invention is to provide the preparation method of the coated DBSA modified carbon nano-tube-polyaniline compound wave-absorbing material of a kind of Mn-Zn ferrite, adding by modified carbon nano-tube, and with the compound of layer/polyaniline conductive polymkeric substance, regulate and control the impedance matching property of composites, overcome the defect that traditional absorbing material density is large.
The present invention is achieved like this, and its preparation method is as follows:
(1) preparation of DBSA modified carbon nano-tube: be that the multi-walled carbon nano-tubes of 20 ~ 30nm joins in the aqueous solution by 1.0g caliber, after ultrasonic disperse 1h, then add 2.0g DBSA, react 2.5h in ice-water bath, carbon nanotube and DBSA mass ratio are 1:2.Extremely neutral through deionized water wash after completion of the reaction, obtain DBSA modified carbon nano-tube after vacuum-drying at 50 DEG C.
(2) preparation of the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite: first according to stoichiometric ratio Mn
xzn
1-xfe
2o
4(X=0.3 ~ 0.9) takes 0.10 ~ 0.30g MnSO respectively
4h
2o, 0.06 ~ 0.42g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, is dissolved in appropriate distilled water, and ultrasonic disperse process 30min dissolves completely, then adds 1.0gDBSA modified carbon nano-tube, then after supersound process 30min, under magnetic stirring apparatus rapid mixing conditions, is titrated to pH value is greater than 8 by 10mol/L NaOH solution.After titration completes, stratification, removes upper clear supernate, and rest part all moves in reactor, reacts 12h under temperature 60 C.Be cooled to room temperature, filter, distilled water wash filter cake to neutral, then uses washing with alcohol 1 ~ 2 time, dry at 70 ~ 80 DEG C, obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.
(3) preparation of the carbon naotube-polyaniline composite material of Mn-Zn ferrite coated DBSA modification: the carbon nanotube taking the coated DBSA modification of Yg (Y=0.05 ~ 0.15) Mn-Zn ferrite respectively, 1mL aniline monomer, add in the there-necked flask filling 35mL0.1mol/L hydrochloric acid soln, ultrasonic disperse 30min, then 2.50g ammonium persulphate is dissolved in 15mL0.1mol/L hydrochloric acid soln, slowly instill in above-mentioned mixing solutions with dropping funnel, 12h is reacted under continuous stirring, filter, use 0.1mol/L hydrochloric acid respectively, deionized water wash product to filtrate is colourless, vacuum-drying 24h at 60 DEG C, obtain the carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of Mn-Zn ferrite.
Observe the particle form of the carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of Mn-Zn ferrite and size with H-600 transmission electron microscope, operating voltage is 75kV.For the carbon naotube-polyaniline mixture (X=0.90, Y=0.15) of the coated DBSA modification of Mn-Zn ferrite, mixture particle diameter is about 100nm.
Measure by the specific conductivity of four point probe conductivity meter to the carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of Mn-Zn ferrite.For the carbon naotube-polyaniline mixture (X=0.30, Y=0.10) of the coated DBSA modification of Mn-Zn ferrite, mixture specific conductivity is 9.59 × 10
-2s/cm.
Magnetism testing is carried out with the carbon naotube-polyaniline composite wave-suction material of vibrating sample magnetometer (VSM) to the coated DBSA modification of Mn-Zn ferrite.For the carbon naotube-polyaniline mixture (X=0.30, Y=0.10) of the coated DBSA modification of Mn-Zn ferrite, test result is: coercive force is 2345.70Oe, and saturation magnetization is 62.95emug
-1, residual magnetization is 39.09emug
-1.
Adopt the reflectivity of carbon naotube-polyaniline composite wave-suction material at 2 ~ 18GHz of the coated DBSA modification of Agilent 8722ES vector network analyzer test Mn-Zn ferrite.With the carbon naotube-polyaniline mixture (X=0.30 of the coated DBSA modification of Mn-Zn ferrite, Y=0.15) be example, test result is: maximum absorption band appears in 14.6GHz place, and peak value is-45dB, and loss of reflectivity value reaches 12.3GHz lower than the absorption band of-10dB is wide.
The carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of the Mn-Zn ferrite prepared by the present invention reaches 12.3 ~ 16.8GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-41 ~-55dB.
Advantage of the present invention:
First the present invention carries out modification to carbon nanotube and reduces reunion, strengthens the dispersiveness of carbon nanotube, according to Mn
xzn
1-xfe
2o
4the stoichiometric of (X=0.3,0.6,0.9), adopts hydrothermal synthesis method to prepare the coated DBSA modified carbon nano-tube of Mn-Zn ferrite; Then with the mass ratio 1 ~ 3:20 of the coated DBSA modified carbon nano-tube of Mn-Zn ferrite and aniline monomer, situ aggregation method is adopted to prepare the carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of Mn-Zn ferrite, this matrix material overcomes the defect that absorbing material density is large, dielectric loss is poor in the past, there is excellent impedance matching and loss characteristic, have broad application prospects in sensing technology, electromagnetic shielding and radar absorption etc.
Embodiment
Below by embodiment, the invention will be further described.
Embodiment 1
(1) be that the multi-walled carbon nano-tubes of 20 ~ 30nm joins in the aqueous solution by 1.0g caliber, after ultrasonic disperse 1h, then add 2.0gDBSA, in ice-water bath, react 2.5h, carbon nanotube and DBSA mass ratio are 1:2.Extremely neutral through deionized water wash after completion of the reaction, vacuum-drying at 50 DEG C, obtains DBSA modified carbon nano-tube.
(2) 0.10g MnSO is taken respectively
4h
2o, 0.42g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, is dissolved in appropriate distilled water, and supersound process 30min dissolves completely, then adds 1.0g DBSA modified carbon nano-tube, again after supersound process 30min, under magnetic stirring apparatus rapid mixing conditions, is titrated to pH value is greater than 8 by 10mol/L NaOH solution.After titration completes, stratification, removes upper clear supernate, and all the other all move in reactor, at 60 DEG C, and reaction 12h.Be cooled to room temperature, filter, distilled water is washed till neutrality, washing with alcohol 1 ~ 2 time, dry at 70 ~ 80 DEG C, obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.
(3) carbon nanotube of the coated DBSA modification of 0.05g Mn-Zn ferrite is taken respectively, 1mL aniline monomer, add in the there-necked flask filling 35mL 0.1mol/L hydrochloric acid soln, ultrasonic disperse 30min, then 2.50g ammonium persulphate is dissolved in 15mL 0.1mol/L hydrochloric acid soln, slowly instill in above-mentioned mixing solutions with dropping funnel, 12h is reacted under continuous stirring, filter, use 0.1mol/L hydrochloric acid respectively, deionized water wash product to filtrate is colourless, vacuum-drying 24h at 60 DEG C, obtain the carbon naotube-polyaniline composite material (X=0.30 of the coated DBSA modification of Mn-Zn ferrite, Y=0.05).Prepared matrix material reaches 14.2GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-41dB.
Embodiment 2
The preparation method of DBSA modified carbon nano-tube is with embodiment 1 step (1).Accurately take 0.10g MnSO
4h
2o, 0.42g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, preparation method, with embodiment 1 step (2), obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.Accurately take the carbon nano tube compound material of the coated DBSA modification of 0.10g Mn-Zn ferrite, 1mL aniline monomer, preparation method is with embodiment 1 step (3), obtain the carbon naotube-polyaniline composite material (X=0.30, Y=0.10) of the coated DBSA modification of Mn-Zn ferrite.Prepared matrix material reaches 13.6GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-42dB.
Embodiment 3
The preparation method of DBSA modified carbon nano-tube is with embodiment 1 step (1).Accurately take 0.10g MnSO
4h
2o, 0.42g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, preparation method, with embodiment 1 step (2), obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.Accurately take the carbon nano tube compound material of the coated DBSA modification of 0.15g Mn-Zn ferrite, 1mL aniline monomer, preparation method is with embodiment 1 step (3), obtain the carbon naotube-polyaniline composite material (X=0.30, Y=0.15) of the coated DBSA modification of Mn-Zn ferrite.Prepared matrix material reaches 12.3GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-45dB.
Embodiment 4
The preparation method of DBSA modified carbon nano-tube is with embodiment 1 step (1).Accurately take 0.20g MnSO
4h
2o, 0.24g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, preparation method, with embodiment 1 step (2), obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.Accurately take the carbon nano tube compound material of the coated DBSA modification of 0.05g Mn-Zn ferrite, 1mL aniline monomer, preparation method is with embodiment 1 step (3), obtain the carbon naotube-polyaniline composite material (X=0.60, Y=0.05) of the coated DBSA modification of Mn-Zn ferrite.Prepared matrix material reaches 16.3GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-46dB.
Embodiment 5
The preparation method of DBSA modified carbon nano-tube is with embodiment 1 step (1).Accurately take 0.20g MnSO
4h
2o, 0.24g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, preparation method, with embodiment 1 step (2), obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.Accurately take the carbon nano tube compound material of the coated DBSA modification of 0.10g Mn-Zn ferrite, 1mL aniline monomer, preparation method is with embodiment 1 step (3), obtain the carbon naotube-polyaniline composite material (X=0.60, Y=0.10) of the coated DBSA modification of Mn-Zn ferrite.Prepared matrix material reaches 15.2GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-49dB.
Embodiment 6
The preparation method of DBSA modified carbon nano-tube is with embodiment 1 step (1).Accurately take 0.20g MnSO
4h
2o, 0.24g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, preparation method, with embodiment 1 step (2), obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.Accurately take the carbon nano tube compound material of the coated DBSA modification of 0.15g Mn-Zn ferrite, 1mL aniline monomer, preparation method is with embodiment 1 step (3), obtain the carbon naotube-polyaniline composite material (X=0.60, Y=0.15) of the coated DBSA modification of Mn-Zn ferrite.Prepared matrix material reaches 14.7GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-50dB.
Embodiment 7
The preparation method of DBSA modified carbon nano-tube is with embodiment 1 step (1).Accurately take 0.30g MnSO
4h
2o, 0.06g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, preparation method, with embodiment 1 step (2), obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.Accurately take the carbon nano tube compound material of the coated DBSA modification of 0.05g Mn-Zn ferrite, 1mL aniline monomer, preparation method is with embodiment 1 step (3), obtain the carbon naotube-polyaniline composite material (X=0.90, Y=0.05) of the coated DBSA modification of Mn-Zn ferrite.Prepared matrix material reaches 16.8GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-48dB.
Embodiment 8
The preparation method of DBSA modified carbon nano-tube is with embodiment 1 step (1).Accurately take 0.30g MnSO
4h
2o, 0.06g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, preparation method, with embodiment 1 step (2), obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.Accurately take the carbon nano tube compound material of the coated DBSA modification of 0.10g Mn-Zn ferrite, 1mL aniline monomer, preparation method is with embodiment 1 step (3), obtain the carbon naotube-polyaniline composite material (X=0.90, Y=0.10) of the coated DBSA modification of Mn-Zn ferrite.Prepared matrix material reaches 15.3GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-51dB.
Embodiment 9
The preparation method of DBSA modified carbon nano-tube is with embodiment 1 step (1).Accurately take 0.30g MnSO
4h
2o, 0.06g Zn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, preparation method, with embodiment 1 step (2), obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite.Accurately take the carbon nano tube compound material of the coated DBSA modification of 0.15g Mn-Zn ferrite, 1mL aniline monomer, preparation method is with embodiment 1 step (3), obtain the carbon naotube-polyaniline composite material (X=0.90, Y=0.15) of the coated DBSA modification of Mn-Zn ferrite.Prepared matrix material reaches 14.8GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-55dB.
Claims (2)
1. a preparation method for the carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of Mn-Zn ferrite, is characterized in that preparation method is as follows:
(1) preparation of DBSA modified carbon nano-tube: be that the multi-walled carbon nano-tubes of 20 ~ 30nm joins in the aqueous solution by 1.0g caliber, after ultrasonic disperse 1h, then add 2.0g DBSA, react 2.5h in ice-water bath, carbon nanotube and DBSA mass ratio are 1:2;
Extremely neutral through deionized water wash after completion of the reaction, obtain DBSA modified carbon nano-tube after vacuum-drying at 50 DEG C;
(2) preparation of the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite: first according to stoichiometric ratio Mn
xzn
1-xfe
2o
4, X=0.3 ~ 0.9 in formula, takes 0.10 ~ 0.30g MnSO respectively
4h
2o, 0.06 ~ 0.42gZn (NO
3)
26H
2o, 1.60g Fe (NO
3)
39H
2o, is dissolved in appropriate distilled water, and ultrasonic disperse process 30min dissolves completely, then adds 1.0g DBSA modified carbon nano-tube, then after supersound process 30min, under magnetic stirring apparatus rapid mixing conditions, is titrated to pH value is greater than 8 by 10mol/L NaOH solution;
After titration completes, stratification, removes upper clear supernate, and rest part all moves in reactor, reacts 12h under temperature 60 C; Be cooled to room temperature, filter, distilled water wash filter cake to neutral, then uses washing with alcohol 1 ~ 2 time, dry at 70 ~ 80 DEG C, obtains the carbon nano tube compound material of the coated DBSA modification of Mn-Zn ferrite;
(3) preparation of the carbon naotube-polyaniline composite material of Mn-Zn ferrite coated DBSA modification: the mass ratio 1 ~ 3:20 controlling the coated DBSA modified carbon nano-tube of Mn-Zn ferrite and aniline monomer, take Yg respectively, wherein Y=0.05 ~ 0.15, the carbon nanotube of the coated DBSA modification of Mn-Zn ferrite, 1mL aniline monomer, add in the there-necked flask filling 35mL 0.1mol/L hydrochloric acid soln, ultrasonic disperse 30min, then 2.50g ammonium persulphate is dissolved in 15mL 0.1mol/L hydrochloric acid soln, slowly instill in above-mentioned mixing solutions with dropping funnel, 12h is reacted under continuous stirring, filter, use 0.1mol/L hydrochloric acid respectively, deionized water wash product to filtrate is colourless, vacuum-drying 24h at 60 DEG C, obtain the carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of Mn-Zn ferrite.
2. the preparation method of the carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of a kind of Mn-Zn ferrite according to claim 1, it is characterized in that: the carbon naotube-polyaniline composite wave-suction material of the coated DBSA modification of prepared Mn-Zn ferrite, prepared matrix material reaches 12.3 ~ 16.8GHz in 2 ~ 18GHz internal reflection rate penalty values lower than the frequency span of-10dB, and minimum reflectance penalty values can reach-41 ~-55dB.
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| CN107487832A (en) * | 2017-05-02 | 2017-12-19 | 四川大学 | A kind of method for removing aldehydes matter in water removal using iron sulphur loading multi-wall carbon nanotubes reinforcing persulfate |
| CN111154259B (en) * | 2019-12-31 | 2022-07-01 | 天长市中德电子有限公司 | Halloysite-cerium doped manganese zinc ferrite composite wave-absorbing material and preparation method thereof |
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| CN102167821A (en) * | 2011-03-24 | 2011-08-31 | 南昌航空大学 | Preparation method of lanthanum-doped barium ferrite-polyaniline composite material microwave absorbent |
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| C06 | Publication | ||
| PB01 | Publication | ||
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