CN103172884A - Preparation method of salicylic acid-modified nickel-zinc ferrite-filled carbon nanotube-polystyrene light absorbing film material - Google Patents
Preparation method of salicylic acid-modified nickel-zinc ferrite-filled carbon nanotube-polystyrene light absorbing film material Download PDFInfo
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- CN103172884A CN103172884A CN2013100612893A CN201310061289A CN103172884A CN 103172884 A CN103172884 A CN 103172884A CN 2013100612893 A CN2013100612893 A CN 2013100612893A CN 201310061289 A CN201310061289 A CN 201310061289A CN 103172884 A CN103172884 A CN 103172884A
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- carbon nanotube
- nickel
- zinc ferrite
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- ointment
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Abstract
The invention provides a preparation method of a salicylic acid-modified nickel-zinc ferrite-filled carbon nanotube-polystyrene light absorbing film material. The preparation method comprises the following steps of: obtaining nickel-zinc ferrite-filled carbon nanotube by adopting a polyvinyl alcohol oxidation opening online filling-hydrothermal method; improving the dispersing capacity of the nickel-zinc ferrite-filled carbon nanotube after the nickel-zinc ferrite-filled carbon nanotube is modified by salicylic acid; and preparing the salicylic acid-modified nickel-zinc ferrite-filled carbon nanotube-polystyrene light absorbing film material by the carbon nanotube and the polystyrene through a solution blending method. The composite is good in conductive performance and electromagnetic performance, and provided with an important application value in the fields of national defense and military, civil electromagnetic protection, microwave shielding and the like.
Description
Technical field
The invention belongs to the anti-electromagnetic radiation field of material preparation, particularly a kind of carbon nanotube of nickel-zinc ferrite filling of Whitfield's ointment modification-polystyrene wave absorbing thin film material preparation method.
Background technology
Ferrite magnetic material has superior magnetic property, but itself and conduction high polymer compound tense often affect the conductivity of matrix material.Carbon nanotube has good conductivity on the one hand, utilizes on the other hand the carbon pipe can play the restriction effect, and electroconductibility that simultaneously can reinforced composite makes composite material concurrent good electric magnetic property.
Therefore, the present invention is by introducing the carbon nanotube through the filling of modifying in p-poly-phenyl ethene matrix, prepare a kind of film that has than the strong electromagnetic wave receptivity, this film can be for the preparation of the radiation prevention film of TV, computer, mobile phone etc., and is significant to the human-body safety preserver.
Summary of the invention
The purpose of this invention is to provide the carbon nanotube that nickel-zinc ferrite that a kind of Whitfield's ointment modifies fills-polystyrene wave absorbing thin film material preparation method, its preparation method is:
(1) 1.0g caliber 10 ~ 225nm multi-walled carbon nano-tubes being joined the 10mL weight ratio is in 30% polyvinyl alcohol solution, after ultrasonic 35min, is heated to 300 ℃ and be incubated 1h, is cooled to room temperature, obtains mixture.Measure than (Ni according to chemical element according to chemical element metering ratio
0.32Zn
0.68O)
1-x(Fe
2O
3)
1+x, wherein X=0.10 ~ 0.40, take 0.05g ~ 0.18g NiSO
46H
2O, 0.11 ~ 0.41g Zn (NO
3)
26H
2O, 4.44g Fe (NO
3)
39H
2O is dissolved in deionized water fully, is dissolved in the 25mL deionized water, then this nitrate solution is poured in above-mentioned mixture, and sealing was placed after 20 days, pour in reactor, 300 ℃ of reaction 6h, cooling, suction filtration, deionized water wash, drying are ground, and obtain the carbon nanotube that Zn ferrite is filled;
(2) preparation of the carbon nanotube of the nickel-zinc ferrite filling of Whitfield's ointment modification: the 1.0g Whitfield's ointment is added in the 40mL deionized water, after magnetic agitation 30min, the carbon nanotube that adds the 1.0g nickel-zinc ferrite to fill, reinforcement stirs 35min, ultrasonic 1h, suction filtration, 60 ℃ of vacuum-drying 24h, grind, obtain the carbon nanotube of the nickel-zinc ferrite filling of Whitfield's ointment modification;
(3) carbon nanotube of the nickel-zinc ferrite filling of Whitfield's ointment modification-polystyrene wave absorbing thin film material preparation: the carbon nanotube that the nickel-zinc ferrite of 0.02 ~ 0.08 gram Whitfield's ointment modification is filled joins in the 50mL tetrahydrofuran solution, ultrasonic 1h, add the 1.0g polystyrene, after continuing ultrasonic 3h, mixing solutions is filmed, 60 ℃ of vacuum-drying 12h obtain the carbon nanotube that nickel-zinc ferrite that Whitfield's ointment modifies fills-polystyrene wave absorbing thin film material.
Film is cut into 5mm * 5mm sheet, and the specific conductivity of the carbon nanotube that the nickel-zinc ferrite of Whitfield's ointment being modified with the four point probe conductivity meter is filled-polystyrene wave absorbing thin film material is measured.The nickel-zinc ferrite of modifying take Whitfield's ointment fill carbon nanotube-polystyrene wave absorbing thin film material (X=0.4) is as example, the mixture specific conductivity is 3.672S/cm.
The carbon nanotube that the nickel-zinc ferrite of Whitfield's ointment being modified with vibrating sample magnetometer (VSM) is filled-polystyrene wave absorbing thin film material carries out magnetism testing.The Zn ferrite of modifying take Whitfield's ointment fill carbon nanotube-polystyrene wave absorbing thin film material (X=0.3) is as example, test result is: coercive force is 2760.32Oe, saturation magnetization is 52.95emug
-1, residual magnetization is 48.29emug
-1
The carbon nanotube that the nickel-zinc ferrite that adopts Agilent 8722ES vector network analyzer test Whitfield's ointment to modify is filled-polystyrene wave absorbing thin film material is at the reflectivity of 2 ~ 18GHz.The carbon nanotube that the nickel-zinc ferrite of modifying take Whitfield's ointment is filled-polystyrene wave absorbing thin film material (X=0.4) is as example, test result is: maximum absorption band appears in the 13.2GHz place, peak value is-42dB, and reflectivity loss value is lower than the wide 15.2GHz that reaches of absorption band of-10dB.
The present invention adopt polyvinyl alcohol oxidation opening fill online-hydrothermal method obtains the carbon nanotube that nickel-zinc ferrite is filled, improve its dispersive ability after Whitfield's ointment is modified, then adopt solution blended process to prepare the carbon nanotube of the nickel-zinc ferrite filling of Whitfield's ointment modification-polystyrene wave absorbing thin film material with polystyrene.This matrix material had both had good electroconductibility, had again magnetic, had important using value in fields such as domestic electromagnetic protection, micro-wave screenings.
Embodiment
The invention will be further described below by embodiment.
Embodiment 1
(1) 1.0g caliber 10 ~ 225nm multi-walled carbon nano-tubes being joined the 10mL weight ratio is in 30% polystyrene solution, after ultrasonic 35min, is heated to 300 ℃ and be incubated 1h, is cooled to room temperature, obtains mixture.Measure than taking 0.05g NiSO according to chemical element according to chemical element metering ratio
46H
2O, 0.11g Zn (NO
3)
26H
2O, 4.44g Fe (NO
3)
39H
2O is dissolved in deionized water fully, be dissolved in the 25mL deionized water, then this nitrate solution poured in above-mentioned mixture in the 25mL deionized water, then this nitrate solution is poured in above-mentioned mixture, sealing was placed after 20 days, pour in reactor, 250 ℃ of reaction 6h, cooling, suction filtration, deionized water wash, drying are ground, and obtain the carbon nanotube that nickel-zinc ferrite is filled.
(2) the 1.0g Whitfield's ointment is added in the 40mL deionized water, after magnetic agitation 30min, the carbon nanotube that adds the 1.0g nickel-zinc ferrite to fill, reinforcement stirs 30min, ultrasonic 1h, suction filtration, 60 ℃ of vacuum-drying 24h grind, and obtain the carbon nanotube of the nickel-zinc ferrite filling of Whitfield's ointment modification.
(3) carbon nanotube that the nickel-zinc ferrite of the 0.02g Whitfield's ointment being modified is filled joins in the 50mL tetrahydrofuran solution, ultrasonic 1h, add the 1.0g polystyrene, after continuing ultrasonic 3h, mixing solutions is filmed, 60 ℃ of vacuum-drying 12h obtain the carbon nanotube that nickel-zinc ferrite that Whitfield's ointment modifies fills-polystyrene wave absorbing thin film material (X=0.3).Prepared matrix material reaches 14.6GHz in 2 ~ 18GHz internal reflection rate loss value lower than the frequency span of-10dB, and minimum reflectance loss value can reach-40dB.
Embodiment 2
The preparation method of the carbon nanotube that the nickel-zinc ferrite that the carbon nanotube that nickel-zinc ferrite is filled, Whitfield's ointment are modified is filled is identical with step (1), (2) of embodiment 1 respectively.The carbon nanotube that the nickel-zinc ferrite of again the 0.04g Whitfield's ointment being modified is filled joins in the 50mL tetrahydrofuran solution, ultrasonic 1h, add the 1.0g polystyrene, after continuing ultrasonic 3h, mixing solutions is filmed, 60 ℃ of vacuum-drying 12h obtain the carbon nanotube that nickel-zinc ferrite that Whitfield's ointment modifies fills-polystyrene wave absorbing thin film material (X=0.3).Prepared matrix material reaches 13.4GHz in 2 ~ 18GHz internal reflection rate loss value lower than the frequency span of-10dB, and minimum reflectance loss value can reach-44dB.
Embodiment 3
The preparation method of the carbon nanotube that the nickel-zinc ferrite that the carbon nanotube that nickel-zinc ferrite is filled, Whitfield's ointment are modified is filled is identical with step (1), (2) of embodiment 1 respectively.The carbon nanotube that the nickel-zinc ferrite of again the 0.06g Whitfield's ointment being modified is filled joins in the 50mL tetrahydrofuran solution, ultrasonic 1h, add the 1.0g polystyrene, after continuing ultrasonic 3h, mixing solutions is filmed, 60 ℃ of vacuum-drying 12h obtain the carbon nanotube that nickel-zinc ferrite that Whitfield's ointment modifies fills-polystyrene wave absorbing thin film material (X=0.3).Prepared matrix material reaches 12.4GHz in 2 ~ 18GHz internal reflection rate loss value lower than the frequency span of-10dB, and minimum reflectance loss value can reach-42dB.
Claims (2)
1. the nickel-zinc ferrite modified of the Whitfield's ointment carbon nanotube of filling-polystyrene wave absorbing thin film material preparation method is characterized in that the preparation method is as follows:
(1) preparation of the nickel-zinc ferrite carbon nanotube of filling: it is in 30% polystyrene solution that 1.0g caliber 10 ~ 225nm multi-walled carbon nano-tubes is joined the 10mL weight ratio, after ultrasonic 35min, be heated to 300 ℃ and be incubated 1h, be cooled to room temperature, obtain mixture, measure than (Ni according to chemical element according to chemical element metering ratio
0.32Zn
0.68O)
1-x(Fe
2O
3)
1+x, wherein X=0.10 ~ 0.40, take 0.05g ~ 0.18g NiSO
46H
2O, 0.11 ~ 0.41g Zn (NO
3)
26H
2O, 4.44g Fe (NO
3)
39H
2O is dissolved in deionized water fully, is dissolved in the 25mL deionized water, then this nitrate solution is poured in above-mentioned mixture, and sealing was placed after 20 days, pour in reactor, 300 ℃ of reaction 6h, cooling, suction filtration, deionized water wash, drying are ground, and obtain the carbon nanotube that Zn ferrite is filled;
(2) preparation of the carbon nanotube of the nickel-zinc ferrite filling of Whitfield's ointment modification: the 1.0g Whitfield's ointment is added in the 40mL deionized water, after magnetic agitation 30min, the carbon nanotube that adds the 1.0g nickel-zinc ferrite to fill, reinforcement stirs 35min, ultrasonic 1h, suction filtration, 60 ℃ of vacuum-drying 24h, grind, obtain the carbon nanotube of the nickel-zinc ferrite filling of Whitfield's ointment modification;
(3) carbon nanotube of the nickel-zinc ferrite filling of Whitfield's ointment modification-polystyrene wave absorbing thin film material preparation: the carbon nanotube that the nickel-zinc ferrite of 0.02 ~ 0.08 gram Whitfield's ointment modification is filled joins in the 50mL tetrahydrofuran solution, ultrasonic 1h, add the 1.0g polystyrene, after continuing ultrasonic 3h, mixing solutions is filmed, 60 ℃ of vacuum-drying 12h obtain the carbon nanotube that nickel-zinc ferrite that Whitfield's ointment modifies fills-polystyrene wave absorbing thin film material.
2. the nickel-zinc ferrite modified of a kind of Whitfield's ointment according to claim 1 carbon nanotube of filling-polystyrene wave absorbing thin film material preparation method, it is characterized in that the carbon nanotube that nickel-zinc ferrite that prepared Whitfield's ointment is modified fills-polystyrene wave absorbing thin film material reaches 12.8-14.8GHz in 2 ~ 18GHz internal reflection rate loss value lower than the frequency span of-10dB, minimum reflectance loss value can reach-35--50dB.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104945759A (en) * | 2014-03-26 | 2015-09-30 | 深圳市润麒麟科技发展有限公司 | Cerium-doped nickel-zinc-ferrite-filled carbon nanotube composite wave-absorbing material and preparation thereof |
| CN106133060A (en) * | 2014-03-25 | 2016-11-16 | 帝斯曼知识产权资产管理有限公司 | Polymer composition, its goods and the method preparing its goods |
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| CN1793421A (en) * | 2005-11-10 | 2006-06-28 | 东华大学 | Process for preparing composite material of carbon nano tube/NiZn ferrite |
| CN101481107A (en) * | 2009-01-23 | 2009-07-15 | 东华大学 | Preparation of nickel-zine ferrite (Ni1-xZnxFe2O4) coated carbon nano-tube magnetic nano composite material |
| CN102924738A (en) * | 2012-10-16 | 2013-02-13 | 南昌航空大学 | Method for preparing carbon nanotube-polystyrene water-absorbing film material filled with salicylic acid-modified zinc ferrite |
-
2013
- 2013-02-27 CN CN2013100612893A patent/CN103172884A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793421A (en) * | 2005-11-10 | 2006-06-28 | 东华大学 | Process for preparing composite material of carbon nano tube/NiZn ferrite |
| CN101481107A (en) * | 2009-01-23 | 2009-07-15 | 东华大学 | Preparation of nickel-zine ferrite (Ni1-xZnxFe2O4) coated carbon nano-tube magnetic nano composite material |
| CN102924738A (en) * | 2012-10-16 | 2013-02-13 | 南昌航空大学 | Method for preparing carbon nanotube-polystyrene water-absorbing film material filled with salicylic acid-modified zinc ferrite |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106133060A (en) * | 2014-03-25 | 2016-11-16 | 帝斯曼知识产权资产管理有限公司 | Polymer composition, its goods and the method preparing its goods |
| CN106133060B (en) * | 2014-03-25 | 2018-09-14 | 帝斯曼知识产权资产管理有限公司 | Polymer composition, its product and the method for preparing its product |
| CN104945759A (en) * | 2014-03-26 | 2015-09-30 | 深圳市润麒麟科技发展有限公司 | Cerium-doped nickel-zinc-ferrite-filled carbon nanotube composite wave-absorbing material and preparation thereof |
| CN104945759B (en) * | 2014-03-26 | 2017-07-18 | 深圳市润麒麟科技发展有限公司 | A kind of cerium dopping nickel-zinc ferrite filling carbon nano-pipe composite wave-suction material and preparation |
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