CN101899234A - Method for preparing glucosyl mesoporous carbon-coated ZnFeO used for electromagnetic wave absorbing coating - Google Patents
Method for preparing glucosyl mesoporous carbon-coated ZnFeO used for electromagnetic wave absorbing coating Download PDFInfo
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- CN101899234A CN101899234A CN2009102630936A CN200910263093A CN101899234A CN 101899234 A CN101899234 A CN 101899234A CN 2009102630936 A CN2009102630936 A CN 2009102630936A CN 200910263093 A CN200910263093 A CN 200910263093A CN 101899234 A CN101899234 A CN 101899234A
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Abstract
The invention discloses a method for preparing glucosyl mesoporous carbon-coated ZnFeO used for electromagnetic wave absorbing coating, which belongs to the preparation process of the electromagnetic wave absorbing coating. In the method, a carbon-coated layer is formed on the surface of Zn ferrite by combining a solvothermal method and high-temperature calcination, which cannot only improve the monodispersion and stability of the ferrite and reduce the density of the ferrite, but also increase the effective absorption of electromagnetic wave, be favorable for expanding absorbing frequency range and fulfill the aims of 'thinness, lightness, wideness and rigidness'. The method is widely used for civil and military use and is more practical.
Description
Technical field
This invention is the technology of preparing that a kind of glucosyl group mesoporous carbon that is used for electromagnetic-absorbing coating coats ZnFeO, belongs to the electromagnetic-absorbing coating preparing technical field.
Technical background
Zinc ferrite material is the bigger material of a kind of loss tangent, not only has higher electrical loss rate, can also be widely used in the electromagnetic-wave absorbent field by magnetic polarization mechanism such as magnetic hysteresis loss, domain wall resonance and the aftereffect loss hertzian wave that absorbs, decays.Usually make compound Zn ferrite by doped with metal elements, in the hope of widening its absorption band, but still can't avoid the big shortcoming of ferrite density.
The dielectric loss type absorbing material of ferrite and light weight carries out compound, not only has multiple microwave absorbing property, and can also further reduce the density of material.Therefore, the simple relatively application prospect of carbon material aspect the lightweight absorbing material of the less and preparation technology of density is very good.Such as report [the Shen G Z that carbon fiber is mixed in the barium ferrite, Xu M, Xu Z.Double-layer microwave absorber based on ferrite and short carbon fiber composites.Mater.Chem.Phys., 2007,105 (2-3): 268-272.], though find that mixing the influence of absorption of sample peak intensity of carbon fiber is also not obvious, the matching thickness of this coating is significantly reduced.Carbon nanotube coats through magneticsubstance or the interior magneticsubstance of filling of pipe, can realize coming the attenuation by absorption hertzian wave by magnetic loss and dielectric loss number of mechanisms, and stronger wide band absorption performance is arranged.But made of carbon nanotubes, purifying process are complicated, also need carry out finishing and could improve filling ratio, just are expected to further strengthen absorption of electromagnetic wave.Shen etc. [Shen Y, Lin Y H, Li M, et al.Adv.Mater., 2007,19 (10): 1418-1422.] adopt simple hydrothermal reaction to prepare the nucleocapsid structure of carbon shell coated with silver, and filling epoxy resin forms matrix material.The carbon shell has played the interface interaction of galactic nucleus and organic matrix, has reduced the tunnel current effect between the contiguous galactic nucleus, makes the unbound electron localization of galactic nucleus.By the Study on dielectric property to the Ag/C epoxy resin composite material, the carbon shell has improved the specific inductivity of matrix material, and simultaneously, by regulating the thickness of carbon shell, specific inductivity also can be effectively controlled.
Ferrite is good to electromagnetic shielding effect, surface at Zn ferrite forms carbon coating layer, not only can improve ferritic monodispersity and stability, reduce ferritic density, and further increase electromagnetic effective absorption, help expanding the absorption frequency range, reach the target of " thin, light, wide, strong ".
Summary of the invention
The objective of the invention is to propose the preparation method that the simple and glucosyl group mesoporous carbon that have an excellent absorption of electromagnetic wave performance of a kind of technology coats ZnFeO.
The present invention comprises following steps: (1), a certain amount of metal-salt is dissolved in 80mL ethylene glycol forms clear solution.To wherein adding 7.2g sodium-acetate and 2g polyoxyethylene glycol PEG2000, after the stirring, reaction mixture is encapsulated into 200 ℃ of solvent thermal reaction 12h in the polytetrafluoroethylkettle kettle; Above-mentioned metal-salt is FeCl
36H
2O and/or ZnCl
2, atoms metal mole total amount is 0.01mol～0.03mol, promptly obtains spherical ZnFeO particle; (2), products therefrom is through separation, washing, drying; (3), get the ZnFeO particle, join in the glucose solution ultrasonic dispersing, 160 ℃ of hydro-thermal reaction 4h in polytetrafluoroethylkettle kettle then; (4), the products therefrom warp, washing, drying are heat-treated in the atmosphere tube type stove of nitrogen protection, thermal treatment temp is from 250 ℃ to 1000 ℃, 1～10 ℃/min of temperature rise rate, target temperature be insulation 2～6h down, promptly obtains the glucosyl group mesoporous carbon and coats ZnFeO.
This invention coats one deck mesoporous carbon outside ferrite nanometer particle, obtain the glucosyl group mesoporous carbon and coat the ZnFeO material.Ferrite is good to electromagnetic shielding effect, surface at Zn ferrite forms carbon coating layer, not only can improve ferritic monodispersity and stability, reduce ferritic density, and further increase electromagnetic effective absorption, help expanding the absorption frequency range, reach the target of " thin, light, wide, strong ".Simple and the glucosyl group mesoporous carbon that obtain of this preparing technique process coats the ZnFeO material and has excellent absorption of electromagnetic wave performance.
Description of drawings
Fig. 1 is the XRD figure spectrum before and after ZnFeO (1: 1) coats.
Fig. 2 is the TEM figure before and after ZnFeO (1: 1) coats: (2-a) ZnFeO (1: 1); (2-b) G-ZnFeO (1: 1).
Fig. 3 is the N2 adsorption desorption curve before and after ZnFeO (1: 1) coats.
Fig. 4 be the reflectivity of different Zn/Fe mol ratio sample ZnFeO-500 with the variation in thickness curve: (4-a) 0: 1; (4-b) 1: 2; (4-c) (1: 1); (4-d) 2: 1; (4-e) 1: 0.
Fig. 5 be the reflectivity of G-ZnFeO (1: 2) different heat treatment temperature sample with the variation in thickness curve: (5-a) 250 ℃; (5-b) 750 ℃; (5-c) 1000 ℃.
Embodiment
Specific embodiment one:
The mol ratio of preparation Zn and Fe is that 0: 1 and glucose coat back 500 ℃ of heat treated glucosyl group mesoporous carbon and coats the ZnFeO materials
(1) 2.70g FeCl
36H
2O is dissolved in 80mL ethylene glycol, forms clear solution.To wherein adding 7.2g sodium-acetate and 2.0g polyoxyethylene glycol PEG2000, vigorous stirring 6h.
(2) reaction mixture is encapsulated in the polytetrafluoroethylkettle kettle 200 ℃ of solvent thermal reaction 12h.
(3) products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.The gained sample is designated as ZnFeO (0: 1), and (0: 1) is the mol ratio of Zn and Fe.
(4) get ZnFeO particle 0.5g, join in the 80mL glucose solution (0.5M) ultrasonic dispersing 30min.
(5) pour mixture into hydrothermal reaction kettle, 160 ℃ of hydro-thermal reaction 4h.The products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.
(6) product is heat-treated in the atmosphere tube type stove of nitrogen protection, 5 ℃/min of temperature rise rate, 500 ℃ are incubated 6h down.
Sample is designated as G-ZnFeO (0: 1)-500, and wherein G is that glucose coats.
G-ZnFeO (0: 1)-500 is made suction ripple specimen with Resins, epoxy by mass ratio at 4: 6, and its reflection loss absorption peak is-7.3dB when thickness of sample is 2mm; Its reflection loss absorption peak reached-28.0dB when thickness of sample was 7mm, less than the wide 3.2GHz that reaches of frequency of-10dB.
Specific embodiment two:
The mol ratio of preparation Zn and Fe is that 1: 2 and glucose coat back 500 ℃ of heat treated glucosyl group mesoporous carbon and coats the ZnFeO materials
(1) 5.40g FeCl
36H
2O and 1.36g ZnCl
2Be dissolved in 80mL ethylene glycol, form clear solution.To wherein adding 7.2g sodium-acetate and 2.0g polyoxyethylene glycol PEG2000, vigorous stirring 6h.
(2) reaction mixture is encapsulated in the polytetrafluoroethylkettle kettle 200 ℃ of solvent thermal reaction 12h.
(3) products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.The gained sample is designated as ZnFeO (1: 2), and (1: 2) is the mol ratio of Zn and Fe.
(4) get ZnFeO particle 0.5g, join in the 80mL glucose solution (0.5M) ultrasonic dispersing 30min.
(5) pour mixture into hydrothermal reaction kettle, 160 ℃ of hydro-thermal reaction 4h.The products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.
(6) product is heat-treated in the atmosphere tube type stove of nitrogen protection, 5 ℃/min of temperature rise rate, 500 ℃ are incubated 6h down.
Sample is designated as G-ZnFeO (1: 2)-500, and wherein G is that glucose coats.
G-ZnFeO (1: 2)-500 is made suction ripple specimen with Resins, epoxy by mass ratio at 4: 6, and its reflection loss absorption peak is-4.3dB when thickness of sample is 2mm; Its reflection loss absorption peak reached-22.2dB when thickness of sample was 7mm, less than the wide 2.4GHz that reaches of frequency of-10dB.
Specific embodiment three:
The mol ratio of preparation Zn and Fe is that 1: 1 and glucose coat back 500 ℃ of heat treated glucosyl group mesoporous carbon and coats the ZnFeO materials
(1) 2.70g FeCl
36H
2O and 1.36g ZnCl
2Be dissolved in 80mL ethylene glycol, form clear solution.To wherein adding 7.2g sodium-acetate and 2.0g polyoxyethylene glycol PEG2000, vigorous stirring 6h.
(2) reaction mixture is encapsulated in the polytetrafluoroethylkettle kettle 200 ℃ of solvent thermal reaction 12h.
(3) products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.The gained sample is designated as ZnFeO (1: 1), and (1: 1) is the mol ratio of Zn and Fe.
(4) get ZnFeO particle 0.5g, join in the 80mL glucose solution (0.5M) ultrasonic dispersing 30min.
(5) pour mixture into hydrothermal reaction kettle, 160 ℃ of hydro-thermal reaction 4h.The products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.
(6) product is heat-treated in the atmosphere tube type stove of nitrogen protection, 5 ℃/min of temperature rise rate, 500 ℃ are incubated 6h down.
Sample is designated as G-ZnFeO (1: 1)-500, and wherein G is that glucose coats.
Present method is simple, and preparation cost is cheap, and the diffraction peak that the ZnFeO of acquisition (1: 1) sample occurs is corresponding with JCPDS standard card (82-1042), is the zinc ferrite of spinel structure.After the glucose hydro-thermal coated, the decolorizing carbon that hydro-thermal generates did not influence the crystalline structure of zinc ferrite.(see figure 1).From Fig. 2-a as can be seen, the nanoparticle that hydro-thermal reaction obtains is the sphere of size than homogeneous, and particle diameter is about 100nm.After the glucose hydro-thermal coated, each nanoparticle was with one deck decolorizing carbon (Fig. 2-c), improved the ZnFeO dispersion of particles outward.The ferrite particle surface irregularity, and by the particle packing balling-up, its BET specific surface area is 20m
2/ g.After the glucose hydro-thermal coated, smooth surface, specific surface area only were 6m
2/ g.The G-ZnFeO (1: 1)-500 that obtains after 500 ℃ of thermal treatment makes by mass ratio with Resins, epoxy and inhales the ripple specimen at 4: 6, and its reflection loss absorption peak is-7.4dB when thickness of sample is 2mm; Its reflection loss absorption peak reached-17.7dB when thickness of sample was 7mm, less than the wide 2.2GHz that reaches of frequency of-10dB.
Specific embodiment four:
The mol ratio of preparation Zn and Fe is that 2: 1 and glucose coat back 500 ℃ of heat treated glucosyl group mesoporous carbon and coats the ZnFeO materials
(1) 2.70g FeCl
36H
2O and 2.72g ZnCl
2Be dissolved in 80mL ethylene glycol, form clear solution.To wherein adding 7.2g sodium-acetate and 2.0g polyoxyethylene glycol PEG2000, vigorous stirring 6h.
(2) reaction mixture is encapsulated in the polytetrafluoroethylkettle kettle 200 ℃ of solvent thermal reaction 12h.
(3) products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.The gained sample is designated as ZnFeO (2: 1), and (2: 1) are the mol ratio of Zn and Fe.
(4) get ZnFeO particle 0.5g, join in the 80mL glucose solution (0.5M) ultrasonic dispersing 30min.
(5) pour mixture into hydrothermal reaction kettle, 160 ℃ of hydro-thermal reaction 4h.The products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.
(6) product is heat-treated in the atmosphere tube type stove of nitrogen protection, 5 ℃/min of temperature rise rate, 500 ℃ are incubated 6h down.
Sample is designated as G-ZnFeO (2: 1), and wherein G is that glucose coats.
G-ZnFeO (2: 1) is made suction ripple specimen with Resins, epoxy by mass ratio at 4: 6, and its reflection loss absorption peak is-4.3dB when thickness of sample is 2mm; Its reflection loss absorption peak reached-22.2dB when thickness of sample was 7mm, less than the wide 2.4GHz that reaches of frequency of-10dB.
Specific embodiment five:
The mol ratio of preparation Zn and Fe is that 1: 0 and glucose coat back 500 ℃ of heat treated glucosyl group mesoporous carbon and coats the ZnFeO materials
(1) 1.36g ZnCl
2Be dissolved in 80mL ethylene glycol, form clear solution.To wherein adding 7.2g sodium-acetate and 2.0g polyoxyethylene glycol PEG2000, vigorous stirring 6h.
(2) reaction mixture is encapsulated in the polytetrafluoroethylkettle kettle 200 ℃ of solvent thermal reaction 12h.
(3) products therefrom is through centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.The gained sample is designated as ZnFeO (1: 0), and (1: 0) is the mol ratio of Zn and Fe.
(4) get ZnFeO particle 0.5g, join in the 80mL glucose solution (0.5M) ultrasonic dispersing 30min.
(5) pour mixture into hydrothermal reaction kettle, 160 ℃ of hydro-thermal reaction 4h.The products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.
(6) product is heat-treated in the atmosphere tube type stove of nitrogen protection, 5 ℃/min of temperature rise rate, 500 ℃ are incubated 6h down.
Sample is designated as G-ZnFeO (1: 0)-500, and wherein G is that glucose coats.
G-ZnFeO (1: 0)-500 is made suction ripple specimen with Resins, epoxy by mass ratio at 4: 6, and its reflection loss absorption peak is-0.8dB when thickness of sample is 2mm; Its reflection loss absorption peak reached-4.9dB when thickness of sample was 7mm.
The absorption of electromagnetic wave performance of the different Zn/Fe mol ratio of table 1 sample ZnFeO-500
Specific embodiment six:
The mol ratio of preparation Zn and Fe is that 1: 2 and glucose coat back 250 ℃ of heat treated glucosyl group mesoporous carbon and coats the ZnFeO materials
(1) 5.40g FeCl
36H
2O and 1.36g ZnCl
2Be dissolved in 80mL ethylene glycol, form clear solution.To wherein adding 7.2g sodium-acetate and 2.0g polyoxyethylene glycol PEG2000, vigorous stirring 6h.
(2) reaction mixture is encapsulated in the polytetrafluoroethylkettle kettle 200 ℃ of solvent thermal reaction 12h.
(3) products therefrom is through centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.The gained sample is designated as ZnFeO (2: 1), and (2: 1) are the mol ratio of Zn and Fe.
(4) get ZnFeO particle 0.5g, join in the 80mL glucose solution (0.5M) ultrasonic dispersing 30min.
(5) pour mixture into hydrothermal reaction kettle, 160 ℃ of hydro-thermal reaction 4h.The products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.
(6) product is heat-treated in the atmosphere tube type stove of nitrogen protection, 1 ℃/min of temperature rise rate, 250 ℃ are incubated 6h down.
Sample is designated as G-ZnFeO (2: 1)-250, and wherein G is that glucose coats.
G-ZnFeO (2: 1)-250 is made suction ripple specimen with Resins, epoxy by mass ratio at 4: 6, and the reflection loss absorption peak of G-ZnFeO when thickness of sample is 2mm (2: 1)-250 is respectively-8.8dB; Its reflection loss absorption peak reached-15.1 when thickness of sample was 7mm.
Specific embodiment seven:
The mol ratio of preparation Zn and Fe is that 1: 1 and glucose coat back 750 ℃ of heat treated glucosyl group mesoporous carbon and coats the ZnFeO materials
(1) 2.70g FeCl
36H
2O and 1.36g ZnCl
2Be dissolved in 80mL ethylene glycol, form clear solution.To wherein adding 7.2g sodium-acetate and 2.0g polyoxyethylene glycol PEG2000, vigorous stirring 6h.
(2) reaction mixture is encapsulated in the polytetrafluoroethylkettle kettle 200 ℃ of solvent thermal reaction 12h.
(3) products therefrom is through centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.The gained sample is designated as ZnFeO (1: 1), and (1: 1) is the mol ratio of Zn and Fe.
(4) get ZnFeO particle 0.5g, join in the 80mL glucose solution (0.5M) ultrasonic dispersing 30min.
(5) pour mixture into hydrothermal reaction kettle, 160 ℃ of hydro-thermal reaction 4h.The products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.Sample is designated as G-ZnFeO (1: 1), and wherein G is that glucose coats.
G-ZnFeO (1: 1)-750 is made suction ripple specimen with Resins, epoxy by mass ratio at 4: 6, and its reflection loss absorption peak is-9.6dB when thickness of sample is 2mm; Its reflection loss absorption peak reached-12.7dB when thickness of sample was 7mm, less than the wide 0.4GHz that reaches of frequency of-10dB.
Specific embodiment eight:
The mol ratio of preparation Zn and Fe is that 1: 2 and glucose coat back 1000 ℃ of heat treated glucosyl group mesoporous carbon and coats the ZnFeO materials
(1) 5.40g FeCl
36H
2O and 1.36g ZnCl
2Be dissolved in 80mL ethylene glycol, form clear solution.To wherein adding 7.2g sodium-acetate and 2.0g polyoxyethylene glycol PEG2000, vigorous stirring 6h.
(2) reaction mixture is encapsulated in the polytetrafluoroethylkettle kettle 200 ℃ of solvent thermal reaction 12h.
(3) products therefrom is through centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.The gained sample is designated as ZnFeO (2: 1), and (2: 1) are the mol ratio of Zn and Fe.
(4) get ZnFeO particle 0.5g, join in the 80mL glucose solution (0.5M) ultrasonic dispersing 30min.
(5) pour mixture into hydrothermal reaction kettle, 160 ℃ of hydro-thermal reaction 4h.The products therefrom centrifugation, distilled water and washing with alcohol three times, 60 ℃ of vacuum-dryings.
(6) product is heat-treated in the atmosphere tube type stove of nitrogen protection, 10 ℃/min of temperature rise rate, 1000 ℃ are incubated 2h down.
Sample is designated as G-ZnFeO (2: 1)-1000, and wherein G is that glucose coats.
G-ZnFeO (2: 1)-1000 is made suction ripple specimen with Resins, epoxy by mass ratio at 4: 6, and the reflection loss absorption peak of G-ZnFeO when thickness of sample is 2mm (2: 1)-1000 is respectively-14.3dB; Its reflection loss absorption peak reached-11.0dB when thickness of sample was 7mm.
The absorption of electromagnetic wave performance of table 2G-ZnFeO (1: 2) different heat treatment temperature sample.
Claims (1)
1. a glucosyl group mesoporous carbon that is used for electromagnetic-absorbing coating coats the preparation method of ZnFeO, it is characterized in that comprising following steps:
(1), a certain amount of metal-salt is dissolved in 80mL ethylene glycol, form clear solution,, after the stirring, reaction mixture is encapsulated into 200 ℃ of solvent thermal reaction 12h in the polytetrafluoroethylkettle kettle to wherein adding 7.2g sodium-acetate and 2g polyoxyethylene glycol PEG2000; Above-mentioned metal-salt is FeCl
36H
2O and/or ZnCl
2, atoms metal mole total amount is 0.01mol～0.03mol, promptly obtains spherical ZnFeO particle;
(2), products therefrom is through separation, washing, drying;
(3), get the ZnFeO particle, join in the glucose solution ultrasonic dispersing, 160 ℃ of hydro-thermal reaction 4h in polytetrafluoroethylkettle kettle then;
(4), the products therefrom warp, washing, drying are heat-treated in the atmosphere tube type stove of nitrogen protection, thermal treatment temp is from 250 ℃ to 1000 ℃, 1～10 ℃/min of temperature rise rate, target temperature be insulation 2～6h down, promptly obtains the glucosyl group mesoporous carbon and coats ZnFeO.
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| CN103159471A (en) * | 2013-03-06 | 2013-06-19 | 哈尔滨工程大学 | Method for preparing carbon-clad spinel ferrite composite material by taking paraffin as carbon source |
| CN105738442A (en) * | 2016-03-25 | 2016-07-06 | 河海大学 | Preparation method for magnetic nanoparticle modified carbon fiber microelectrode and application thereof |
| CN107142080A (en) * | 2017-05-02 | 2017-09-08 | 南京航空航天大学 | A kind of adjustable CoNi/ porous carbons microwave absorption of ratio and preparation method thereof |
| CN108102393A (en) * | 2017-12-20 | 2018-06-01 | 合肥工业大学 | A kind of preparation method of the electromagnetic wave absorbent material based on ferrite solid waste |
| CN108102393B (en) * | 2017-12-20 | 2020-06-26 | 合肥工业大学 | Preparation method of electromagnetic wave absorbing material based on ferrite solid waste |
| CN109453739A (en) * | 2018-10-15 | 2019-03-12 | 南京农业大学 | Ni/Fe3O4@C composite and its preparation method and application |
| CN109796802A (en) * | 2018-12-07 | 2019-05-24 | 浙江传化涂料有限公司 | A kind of preparation method and applications of the hollow carbosphere of carbon coating titanium dioxide |
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Application publication date: 20101201 |