CN102924714A - Method for preparing carbon nanotube-polyaniline composite wave-absorbing material filled with SDBS (Sodium Dodecyl Benzene Sulfonate)-modified manganese-zinc ferrite - Google Patents
Method for preparing carbon nanotube-polyaniline composite wave-absorbing material filled with SDBS (Sodium Dodecyl Benzene Sulfonate)-modified manganese-zinc ferrite Download PDFInfo
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- CN102924714A CN102924714A CN 201210390020 CN201210390020A CN102924714A CN 102924714 A CN102924714 A CN 102924714A CN 201210390020 CN201210390020 CN 201210390020 CN 201210390020 A CN201210390020 A CN 201210390020A CN 102924714 A CN102924714 A CN 102924714A
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Abstract
The invention provides a method for preparing a carbon nanotube-polyaniline composite wave-absorbing material filled with SDBS (Sodium Dodecyl Benzene Sulfonate)-modified manganese-zinc ferrite. The method comprises the following steps of: preparing a carbon nanotube filled manganese-zinc ferrite by adopting a potassium dichromate oxidizing opening online filling-high temperature method; modifying through SDBS for improving the dispersing power of the carbon nanotube; and preparing a carbon nanotube-polyaniline composite material filled with SDBS-modified manganese-zinc ferrite from an aniline monomer by adopting an in-situ polymerization method. The composite material has high electromagnetic property, and has important application values in the fields of national defense stealth, civil electromagnetic protection, microwave shield and the like.
Description
Technical field
The invention belongs to the electromagnetic wave absorbent material preparation field, particularly a kind of preparation method of carbon naotube-polyaniline composite wave-suction material of Mn-Zn ferrite filling of SDBS modification.
Background technology
Polyaniline mainly reaches by electrical loss electromagnetic absorption, is difficult to obtain satisfied effect, the effective way that should seek to realize the polyaniline high conductivity or have function solenoid concurrently.Therefore, the present invention from the angle of composite materials adopt the potassium dichromate oxidation opening fill online-pyroprocess obtains the carbon nanotube that Mn-Zn ferrite is filled, through the SDBS(Sodium dodecylbenzene sulfonate) improve its dispersive ability after modifying, adopt situ aggregation method to prepare the carbon naotube-polyaniline composite material of the Mn-Zn ferrite filling that SDBS modifies with aniline monomer again.
Summary of the invention
The purpose of this invention is to provide the preparation method of the carbon naotube-polyaniline composite wave-suction material that Mn-Zn ferrite that a kind of SDBS modifies fills, its preparation method is:
(1) preparation of the carbon nanotube of Mn-Zn ferrite filling: be Mn according to chemical element metering ratio
0.5Zn
0.5Fe
2O
4Take by weighing 0.85g MnSO
4H
2O, 1.49g Zn (NO
3)
26H
2O, 8.08g Fe (NO
3)
39H
2O is dissolved in the 30mL deionized water, add 1.0g caliber 20 ~ 30nm multi-walled carbon nano-tubes, 20mL 1.0mol/L potassium bichromate, reinforcement stirs 30min, 90 ℃ of water-bath 4h, suction filtration, washing, after the drying, put into quartz boat, the tube-type atmosphere furnace of packing into passes into argon gas, gas flow 0.2L/min, heat-up rate is 10 ℃/min, is warming up to 950 ℃ and keeps 2h, naturally cools to room temperature, after being about 7 with deionized water rinsing to pH, again filters product, 50 ℃ of vacuum-dryings are ground, and obtain the carbon nanotube that Mn-Zn ferrite is filled.
(2) preparation of the carbon nanotube of the Mn-Zn ferrite filling of SDBS modification: 1.0g Sodium dodecylbenzene sulfonate (SDBS) is added in the 60mL deionized water, behind the magnetic agitation 30min, add the carbon nanotube that the 1.0g Mn-Zn ferrite is filled, reinforcement stirs 30min, ultrasonic 1h, suction filtration, 60 ℃ of vacuum-drying 24h, grind, obtain the carbon nanotube of the Mn-Zn ferrite filling of SDBS modification.
(3) in the carbon nanotube adding 20mL 1mol/L hydrochloric acid soln that the preparation of the carbon naotube-polyaniline composite material of the Mn-Zn ferrite filling of SDBS modification: with Xg(X=0.20 ~ 0.80) Mn-Zn ferrite of SDBS modification is filled, behind the ultrasonic 1h, add the 1.0mL aniline monomer, after ice-water bath stirs 10min, continue to stir the lower 10mL 1mol/L ammonium persulfate solution that slowly splashes into, continue to stir 3h, suction filtration, deionized water wash 3 ~ 4 times, 60 ℃ of lower vacuum-drying 12h obtain the carbon naotube-polyaniline composite wave-suction material that Mn-Zn ferrite that SDBS modifies is filled.
With the H-600 transmission electron microscope particle form and the size of the carbon naotube-polyaniline composite wave-suction material of the Mn-Zn ferrite filling of SDBS modification are observed, operating voltage is 75kV.The carbon naotube-polyaniline mixture (X=0.20) that the Mn-Zn ferrite of modifying take SDBS is filled is as example, and the mixture mean diameter is about 50nm.
With the four point probe conductivity meter specific conductivity of the carbon naotube-polyaniline composite wave-suction material of the Mn-Zn ferrite filling of SDBS modification is measured.The carbon naotube-polyaniline mixture (X=0.40) that the Mn-Zn ferrite of modifying take SDBS is filled is as example, and the mixture specific conductivity is 1.876S/cm.
The carbon naotube-polyaniline composite wave-suction material of the Mn-Zn ferrite of SDBS modification being filled with vibrating sample magnetometer (VSM) carries out magnetism testing.The carbon naotube-polyaniline mixture (X=0.60) that the Mn-Zn ferrite of modifying take SDBS is filled is as example, and test result is: coercive force is 3556.42Oe, and saturation magnetization is 72.92emug
-1, residual magnetization is 68.09emug
-1
The carbon naotube-polyaniline composite wave-suction material that the Mn-Zn ferrite that adopts Agilent 8722ES vector network analyzer test SDBS to modify is filled is at the reflectivity of 2 ~ 18GHz.The carbon naotube-polyaniline mixture (X=0.80) that the Mn-Zn ferrite of modifying take SDBS is filled is as example, and test result is: maximum absorption band appears in the 9.8GHz place, and peak value is-48dB, and reflectivity loss value is lower than-the wide 11.4GHz of reaching of absorption band of 10dB.
The present invention adopt the potassium dichromate oxidation opening fill online-pyroprocess obtains the carbon nanotube that Mn-Zn ferrite is filled, after Sodium dodecylbenzene sulfonate (SDBS) is modified, improve its dispersive ability, adopt situ aggregation method to prepare the carbon naotube-polyaniline composite material of the Mn-Zn ferrite filling of SDBS modification with aniline monomer again.This matrix material has good electromagnetic performance, and the field such as, domestic electromagnetic protection stealthy in national defence, micro-wave screening has important using value.
Embodiment
The invention will be further described below by embodiment.
Embodiment 1
(1) compares Mn according to the chemical element metering
0.5Zn
0.5Fe
2O
4Take by weighing 0.85g MnSO
4H
2O, 1.49g Zn (NO
3)
26H
2O, 8.08g Fe (NO
3)
39H
2O is dissolved in the 30mL deionized water, add 1.0g caliber 20 ~ 30nm multi-walled carbon nano-tubes, 20mL 1.0mol/L potassium bichromate, reinforcement stirs 30min, 90 ℃ of water-bath 4h, suction filtration, washing, after the drying, put into quartz boat, the tube-type atmosphere furnace of packing into passes into argon gas, gas flow 0.2L/min, heat-up rate is 10 ℃/min, is warming up to 950 ℃ and keeps 2h, naturally cools to room temperature, after being about 7 with deionized water rinsing to pH, again filters product, 50 ℃ of vacuum-dryings are ground, and obtain the carbon nanotube that Mn-Zn ferrite is filled.
(2) 1.0g Sodium dodecylbenzene sulfonate (SDBS) is added in the 60mL deionized water, behind the magnetic agitation 30min, add the carbon nanotube that the 1.0g Mn-Zn ferrite is filled, reinforcement stirs 30min, ultrasonic 1h, suction filtration, 60 ℃ of vacuum-drying 24h, grind, obtain the carbon nanotube of the Mn-Zn ferrite filling of SDBS modification.
(3) carbon nanotube that the Mn-Zn ferrite of 0.20g SDBS being modified is filled adds in the 20mL 1mol/L hydrochloric acid soln, behind the ultrasonic 1h, add the 1.0mL aniline monomer, after ice-water bath stirs 10min, continue to stir the lower 10mL 1mol/L ammonium persulfate solution that slowly splashes into, continue to stir 3h, suction filtration, deionized water wash 3 ~ 4 times, 60 ℃ of lower vacuum-drying 12h obtain the carbon naotube-polyaniline composite wave-suction material (X=0.20) that Mn-Zn ferrite that SDBS modifies is filled.Prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 14.2GHz, and minimum reflectance loss value can reach-45dB.
Embodiment 2
The preparation method of the carbon nanotube that the Mn-Zn ferrite that the carbon nanotube that Mn-Zn ferrite is filled, SDBS modify is filled is respectively with routine 1(1), (2).Take by weighing the carbon nanotube that Mn-Zn ferrite that 0.40g SDBS modifies is filled, the preparation method is with routine 1(3), make the carbon naotube-polyaniline composite wave-suction material (X=0.40) that Mn-Zn ferrite that SDBS modifies is filled.Prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 13.4GHz, and minimum reflectance loss value can reach-46dB.
Embodiment 3
The preparation method of the carbon nanotube that the Mn-Zn ferrite that the carbon nanotube that Mn-Zn ferrite is filled, SDBS modify is filled is respectively with routine 1(1), (2).Take by weighing the carbon nanotube that Mn-Zn ferrite that 0.60g SDBS modifies is filled, the preparation method is with routine 1(3), make the carbon naotube-polyaniline composite wave-suction material (X=0.60) that Mn-Zn ferrite that SDBS modifies is filled.Prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 12.3GHz, and minimum reflectance loss value can reach-47dB.
Embodiment 4
The preparation method of the carbon nanotube that the Mn-Zn ferrite that the carbon nanotube that Mn-Zn ferrite is filled, SDBS modify is filled is respectively with routine 1(1), (2).Take by weighing the carbon nanotube that Mn-Zn ferrite that 0.80g SDBS modifies is filled, the preparation method is with routine 1(3), make the carbon naotube-polyaniline composite wave-suction material (X=0.80) that Mn-Zn ferrite that SDBS modifies is filled.Prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 11.4GHz, and minimum reflectance loss value can reach-48dB.
Claims (2)
1. the preparation method of the carbon naotube-polyaniline composite wave-suction material of the Mn-Zn ferrite filling of a SDBS modification is characterized in that, the preparation method is as follows:
(1) preparation of the carbon nanotube of Mn-Zn ferrite filling: be Mn according to chemical element metering ratio
0.5Zn
0.5Fe
2O
4Take by weighing 0.85g MnSO
4H
2O, 1.49g Zn (NO
3)
26H
2O, 8.08g Fe (NO
3)
39H
2O is dissolved in the 30mL deionized water, add 1.0g caliber 20 ~ 30nm multi-walled carbon nano-tubes, 20mL 1.0mol/L potassium bichromate, reinforcement stirs 30min, 90 ℃ of water-bath 4h, suction filtration, washing, after the drying, put into quartz boat, the tube-type atmosphere furnace of packing into passes into argon gas, gas flow 0.2L/min, heat-up rate is 10 ℃/min, is warming up to 950 ℃ and keeps 2h, naturally cools to room temperature, after being about 7 with deionized water rinsing to pH, again filters product, 50 ℃ of vacuum-dryings are ground, and obtain the carbon nanotube that Mn-Zn ferrite is filled;
(2) preparation of the carbon nanotube of the Mn-Zn ferrite filling of SDBS modification: 1.0gSDBS is added in the 60mL deionized water, behind the magnetic agitation 30min, add the carbon nanotube that the 1.0g Mn-Zn ferrite is filled, reinforcement stirs 30min, ultrasonic 1h, suction filtration, 60 ℃ of vacuum-drying 24h, grind, obtain the carbon nanotube of the Mn-Zn ferrite filling of SDBS modification;
(3) preparation of the Mn-Zn ferrite modified of the SDBS carbon naotube-polyaniline composite material of filling: the carbon nanotube that the Mn-Zn ferrite that 0.20 ~ 0.80 gram SDBS is modified is filled adds in the 20mL 1mol/L hydrochloric acid soln, behind the ultrasonic 1h, add the 1.0mL aniline monomer, after ice-water bath stirs 10min, continue to stir the lower 10mL 1mol/L ammonium persulfate solution that slowly splashes into, continue to stir 3h, suction filtration, deionized water wash 3 ~ 4 times, 60 ℃ of lower vacuum-drying 12h obtain the carbon naotube-polyaniline composite wave-suction material that Mn-Zn ferrite that SDBS modifies is filled.
2. the Mn-Zn ferrite modified of the prepared SDBS of preparation method of the Mn-Zn ferrite modified of a kind of SDBS according to claim 1 carbon naotube-polyaniline composite wave-suction material of the filling carbon naotube-polyaniline composite material of filling, prepared matrix material is lower than in 2 ~ 18GHz internal reflection rate loss value-and the frequency span of 10dB reaches 11.4-14.2GHz, and minimum reflectance loss value can reach-45--48dB.
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CN103122066A (en) * | 2013-02-27 | 2013-05-29 | 南昌航空大学 | Preparation method of SDBS (sodium dodecyl benzene sulfonate) modified manganese-copper-cobalt ferrite filled carbon nanotube-polypyrrole composite wave absorbing material |
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CN111138184A (en) * | 2019-12-31 | 2020-05-12 | 天长市中德电子有限公司 | Carbon composite cerium-doped manganese-zinc ferrite wave-absorbing material and preparation method thereof |
CN111471342A (en) * | 2020-04-24 | 2020-07-31 | 郑逢平 | Manganese-zinc ferrite-carbon nanotube grafted polyaniline wave-absorbing coating and preparation method thereof |
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CN103122066A (en) * | 2013-02-27 | 2013-05-29 | 南昌航空大学 | Preparation method of SDBS (sodium dodecyl benzene sulfonate) modified manganese-copper-cobalt ferrite filled carbon nanotube-polypyrrole composite wave absorbing material |
CN103122144A (en) * | 2013-02-27 | 2013-05-29 | 南昌航空大学 | Preparation method of DBSA (dodecyl benzene sulfonic acid) modified lanthanum doped barium ferrite filled carbon nano-tube-poly-o-methylaniline composite wave-absorbing material |
CN103122126A (en) * | 2013-02-27 | 2013-05-29 | 南昌航空大学 | Preparation method of DBSA (dodecyl benzene sulfonic acid) modified manganese copper ferrite filled carbon nano-tube-polythiophene composite wave-absorbing material |
CN105153678A (en) * | 2015-10-13 | 2015-12-16 | 中国人民解放军***武汉总医院 | Preparation of carbon nanotube-conducting high-polymer material/ferrite composite polyurethane |
CN111138184A (en) * | 2019-12-31 | 2020-05-12 | 天长市中德电子有限公司 | Carbon composite cerium-doped manganese-zinc ferrite wave-absorbing material and preparation method thereof |
CN111471342A (en) * | 2020-04-24 | 2020-07-31 | 郑逢平 | Manganese-zinc ferrite-carbon nanotube grafted polyaniline wave-absorbing coating and preparation method thereof |
CN112537762A (en) * | 2020-12-22 | 2021-03-23 | 中北大学 | Refining and dispersing method of battery positive electrode material |
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Application publication date: 20130213 |