CN107828372A - A kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption - Google Patents
A kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption Download PDFInfo
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- CN107828372A CN107828372A CN201711161622.2A CN201711161622A CN107828372A CN 107828372 A CN107828372 A CN 107828372A CN 201711161622 A CN201711161622 A CN 201711161622A CN 107828372 A CN107828372 A CN 107828372A
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Abstract
The present invention relates to a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption, belong to absorbing material technical field.The present invention is using graphene as matrix material, by chemical coprecipitation on graphene oxide sheet, simultaneous oxidation graphite is heat-treated by original position, the mixed binding of Conjugate ferrite and graphene graphene big specific surface area, excellent electric conductivity, the preferably more avtive spot of pliability and ferrite, outstanding magnetic characteristic and good chemical stability, and effectively improve the stacked structure between graphene layer, be made has dielectric loss and the absorbing material of magnetic loss simultaneously to electromagnetic wave, the present invention passes through the composite mixed bismuth oxide of graphene/Conjugate ferrite and aluminum oxide, significantly improve ferritic thermal shock resistance, simultaneously in ferrite surfaces coated silica, isolation protection is carried out to Conjugate ferrite, and cooperate with the high thermal conductivity of graphene, further improve the resistance to elevated temperatures of absorbing material.
Description
Technical field
The present invention relates to a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption, belong to absorbing material skill
Art field.
Background technology
Electromagnetic wave absorbent material is a kind of electromagnetic wave that can be decayed by the absorption of itself, reflection, scatters and transmits
All functional materials of very little.Its general principle is to convert electromagnetic waves into the energy of the other forms such as heat energy, electric energy or mechanical energy
And consume.It can be divided into following fundamental type according to the operation principle of electromagnetic wave absorbent material：Complex permeability and complex dielectric permittivity
Of substantially equal absorbing material；Quarter-wave " resonance " absorbing material；Impedance transition mechanism " wideband " absorbing material；Decay surface
The thin layer absorbing material of electric current.
With the rapid development of modern radar and microwave electron technology, electromagnetic wave is increasing in the intensity of spatial distribution,
The wavelength of distribution also even extends to broader wave band from metric wave to millimeter wave, and electromagnetic wave absorbent material application field is also increasingly
Extensively, while to absorbing material higher requirement is proposed, is embodied in following several respects：Thickness of thin, light weight, absorption band
Wide, absorbability is strong and intellectuality etc..
Absorbing material is mainly made up of absorbent and matrix material, and absorbent has been to absorb the thing with reflection electromagnetic wave effect
Matter, conventional has ferrite, carbonyl iron, conduction high polymer etc..And matrix material is the carrier of absorbent, it can carry and disperse
Absorbent, and itself there is certain mechanical property, such as rubber, flexible polyurethane foams agent, hard styrofoam.
From the operation principle of absorbing material, the wave-sucking performance of absorbing material and the absorbability of absorbent have substantial connection, therefore,
The development and exploitation of absorbent are the important research directions in absorbing material field.
Radio-radar absorber is broadly divided into resistor-type, dielectric type and magnetizing mediums type by its loss mechanism.With e-mail
The development of industry is ceased, electromagnetic pollution has become the problem of very serious.Absorbing material can absorb and decay incident electromagnetic wave, and lead to
The electromagnetic energy such as dielectric loss, vortex and magnetic hysteresis be flexible of absorbent is crossed to dissipate into heat energy or make electromagnetic wave because of interference
And disappear.It is valued by people in terms of civil and military.But most of absorbing material developed at present can only compared with
Used at low temperature.If ferrite, hydroxy iron powder class absorbent are when temperature environment is higher than its Curie temperature, permeability
Decline can cause the deterioration of absorbing property；It is oxidized when C-C classes absorbing material is due to high temperature and loses absorbing property.This is just full
The foot not demand of weaponry high-temperature component stealthyization, so must develop can bear high temperature and temperature shock for a long time
Absorbing material.
The content of the invention
The technical problems to be solved by the invention：It can only at a lower temperature be used for current absorbing material, work as temperature
A kind of the problem of degree environment is when being higher than its Curie temperature, and the decline of permeability can cause absorbing property to deteriorate, there is provided silicon
The preparation method of coating-codoping Conjugate ferrite microwave absorption.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Take graphene oxide to add ultrasonic disperse in deionized water, add urea, be well mixed to obtain graphene dispersing solution；
（2）Cobalt chloride, frerrous chloride are taken, adds in hydrochloric acid and is well mixed, then under nitrogen atmosphere, be added dropwise to 1~2mL/min
In graphene dispersing solution, and be heated to 90~100 DEG C reaction 2~3h, stand 10~15h after filtration washing dry, obtain graphene/
Conjugate ferrite；
（3）Graphene/Conjugate ferrite, bismuth oxide, aluminum oxide, absolute ethyl alcohol are taken, is fitted into 20~24h of ball milling in ball mill, ball milling
20~30min of ultrasonic disperse in ethanol solution is transferred to after end, obtains codope Conjugate ferrite dispersion liquid；
（4）Tetraethyl orthosilicate is added dropwise into codope Conjugate ferrite dispersion liquid, ammoniacal liquor is added dropwise after well mixed, after stirring 8~10h
Filtration washing is dried, and obtains silicon coating-codoping Conjugate ferrite microwave absorption.
Step（1）The graphene oxide and the mass ratio of deionized water are 1：250~1：1000, the amount of urea is
3.6~14.4 times of graphene oxide quality.
Step（2）The cobalt chloride, the mol ratio of frerrous chloride are 1：2, frerrous chloride dosage is graphene oxide quality
2.5~10 times.
Step（3）Graphene/the Conjugate ferrite, bismuth oxide, aluminum oxide, the parts by weight of absolute ethyl alcohol are 10~20 parts
Graphene/Conjugate ferrite, 0.06~0.12 part of bismuth oxide, 0.12~0.24 part of aluminum oxide, 5~10 parts of absolute ethyl alcohols.
Step（3）The mass fraction of the ethanol solution is 10%, and dosage is the 10~40 of graphene/Conjugate ferrite quality
Times.
Step（4）The dosage of the tetraethyl orthosilicate is the 25~100% of graphene/Conjugate ferrite quality.
Step（4）The mass fraction of the ammoniacal liquor is 25%, and dosage is 1~4 times of graphene/Conjugate ferrite quality.
Compared with other method, advantageous effects are the present invention：
（1）The present invention is with the loose structure with high specific surface area and opening, good pliability and chemically and thermally steady
Qualitatively graphene is matrix material, by chemical coprecipitation on graphene oxide sheet, simultaneous oxidation graphite by in-situ heat also
The mixed binding of original, Conjugate ferrite and graphene graphene big specific surface area, excellent electric conductivity, preferable pliability and
The more avtive spot of ferrite, outstanding magnetic characteristic and good chemical stability, and effectively improve graphene layer
Between stacked structure, be made to electromagnetic wave simultaneously there is dielectric loss and the absorbing material of magnetic loss；
（2）The present invention is significantly improved ferritic resistance to by the composite mixed bismuth oxide of graphene/Conjugate ferrite and aluminum oxide
Thermal shock resistance properties, while in ferrite surfaces coated silica, isolation protection is carried out to Conjugate ferrite, and cooperate with graphene
High thermal conductivity, further improve the resistance to elevated temperatures of absorbing material.
Embodiment
5~10g graphene oxides are taken, are added in 2.5~5.0L deionized waters, 1~2h is disperseed with 300W ultrasonic echographies,
36~72g urea is added, 30~40min is stirred with 300~400r/min, graphene dispersing solution is obtained, takes 0.1~0.2mol chlorine
Change cobalt, 0.2~0.4mol frerrous chlorides, it is in 0.1% hydrochloric acid to add 200~300mL mass fractions, is stirred with 300~400r/min
30~40min is mixed, then under nitrogen atmosphere, is added dropwise to 1~2mL/min in graphene dispersing solution, continues stirring until and drips
Finish, be again heated to 90~100 DEG C of 2~3h of reaction, filter to obtain filter residue after standing 10~15h, filter residue 3~5 is washed with deionized
It is placed in after secondary in drying box, 4~6h is dried at 60~80 DEG C, graphene/Conjugate ferrite is obtained, takes 10~20g graphenes/ferro-cobalt
Oxysome, 0.06~0.12g bismuth oxides, 0.12~0.24g aluminum oxide, 5~10g absolute ethyl alcohols, it is fitted into ball mill, with 350~
400r/min 20~24h of ball milling, ball milling is transferred to 200~400g mass fractions after terminating be in 10% ethanol solution, with 300W ultrasounds
Ripple 20~30min of ultrasonic disperse, codope Conjugate ferrite dispersion liquid is obtained, takes 5~10g tetraethyl orthosilicates, with 1~2mL/min drops
Add in codope Conjugate ferrite dispersion liquid, 20~30min is stirred with 300~400r/min, then 10 are added dropwise with 1~2mL/min
~20g mass fractions are 25% ammoniacal liquor, filter to obtain filter cake after persistently stirring 8~10h, filter cake is washed with deionized to cleaning solution
In neutrality, then it is transferred in drying box, 4~6h is dried at 60~80 DEG C, obtains silicon coating-codoping Conjugate ferrite microwave absorption.
Example 1
5g graphene oxides are taken, are added in 2.5L deionized waters, 1h is disperseed with 300W ultrasonic echographies, adds 36g urea, with
300r/min stirs 30min, obtains graphene dispersing solution, takes 0.1mol cobalt chlorides, 0.2mol frerrous chlorides, adds 200mL mass
Fraction is in 0.1% hydrochloric acid, stirs 30min with 300r/min, then under nitrogen atmosphere, graphene dispersion is added dropwise to 1mL/min
In liquid, continue stirring until and be added dropwise, be again heated to 90 DEG C of reaction 2h, filter to obtain filter residue after standing 10h, be washed with deionized
It is placed in after filter residue 3 times in drying box, 4h is dried at 60 DEG C, graphene/Conjugate ferrite is obtained, takes 10g graphenes/Conjugate ferrite,
0.06g bismuth oxides, 0.12g aluminum oxide, 5g absolute ethyl alcohols, it is fitted into ball mill, with 350r/min ball milling 20h, after ball milling terminates
200g mass fractions are transferred in 10% ethanol solution, to disperse 20min with 300W ultrasonic echographies, obtain codope Conjugate ferrite point
Dispersion liquid, 5g tetraethyl orthosilicates are taken, be added dropwise in codope Conjugate ferrite dispersion liquid with 1mL/min, stirred with 300r/min
20min, then 10g mass fractions are added dropwise as 25% ammoniacal liquor using 1mL/min, filter cake is filtered to obtain after persistently stirring 8h, is washed with deionized water
Filter cake is washed to cleaning solution in neutrality, then is transferred in drying box, 4h is dried at 60 DEG C, obtains silicon coating-codoping Conjugate ferrite microwave
Absorbent.
Example 2
8g graphene oxides are taken, are added in 3.5L deionized waters, 1h is disperseed with 300W ultrasonic echographies, adds 54g urea, with
350r/min stirs 35min, obtains graphene dispersing solution, takes 0.1mol cobalt chlorides, 0.3mol frerrous chlorides, adds 250mL mass
Fraction is in 0.1% hydrochloric acid, stirs 35min with 350r/min, then under nitrogen atmosphere, graphene dispersion is added dropwise to 1mL/min
In liquid, continue stirring until and be added dropwise, be again heated to 95 DEG C of reaction 2h, filter to obtain filter residue after standing 12h, be washed with deionized
It is placed in after filter residue 4 times in drying box, 5h is dried at 70 DEG C, graphene/Conjugate ferrite is obtained, takes 15g graphenes/Conjugate ferrite,
0.09g bismuth oxides, 0.18g aluminum oxide, 8g absolute ethyl alcohols, it is fitted into ball mill, with 380r/min ball milling 22h, after ball milling terminates
300g mass fractions are transferred in 10% ethanol solution, to disperse 25min with 300W ultrasonic echographies, obtain codope Conjugate ferrite point
Dispersion liquid, 8g tetraethyl orthosilicates are taken, be added dropwise in codope Conjugate ferrite dispersion liquid with 1mL/min, stirred with 350r/min
25min, then 15g mass fractions are added dropwise as 25% ammoniacal liquor using 1mL/min, filter cake is filtered to obtain after persistently stirring 9h, is washed with deionized water
Filter cake is washed to cleaning solution in neutrality, then is transferred in drying box, 5h is dried at 70 DEG C, obtains silicon coating-codoping Conjugate ferrite microwave
Absorbent.
Example 3
10g graphene oxides are taken, are added in 5.0L deionized waters, 2h is disperseed with 300W ultrasonic echographies, adds 72g urea,
40min is stirred with 400r/min, obtains graphene dispersing solution, 0.2mol cobalt chlorides is taken, 0.4mol frerrous chlorides, adds 300mL matter
It is in 0.1% hydrochloric acid to measure fraction, and 40min is stirred with 400r/min, then under nitrogen atmosphere, graphene point is added dropwise to 2mL/min
In dispersion liquid, continue stirring until and be added dropwise, be again heated to 100 DEG C of reaction 3h, filter to obtain filter residue after standing 15h, use deionized water
It is placed in after washing filter residue 5 times in drying box, 6h is dried at 80 DEG C, graphene/Conjugate ferrite is obtained, takes 20g graphenes/ferro-cobalt oxygen
Body, 0.12g bismuth oxides, 0.24g aluminum oxide, 10g absolute ethyl alcohols, it is fitted into ball mill, with 400r/min ball milling 24h, ball milling knot
400g mass fractions are transferred to after beam in 10% ethanol solution, to disperse 30min with 300W ultrasonic echographies, obtaining codope ferro-cobalt oxygen
Dispersion liquid, 10g tetraethyl orthosilicates are taken, be added dropwise in codope Conjugate ferrite dispersion liquid with 2mL/min, stirred with 400r/min
30min, then 20g mass fractions are added dropwise as 25% ammoniacal liquor using 2mL/min, filter cake is filtered to obtain after persistently stirring 10h, uses deionized water
Filter cake is washed to cleaning solution in neutrality, then is transferred in drying box, 6h is dried at 80 DEG C, it is micro- to obtain silicon coating-codoping Conjugate ferrite
Wave absorbent.
Reference examples：The microwave absorption of Jiangsu company production.
The microwave absorption of example and reference examples is detected, specific detection is as follows：
Using the dielectric constant of Agilent Technologies E8362B vector network tester test samples, the frequency of test
Rate scope is 2-18GHz.It is as follows to measure Sample Preparation Procedure：Determinand and paraffin are heated with certain mass ratio or volume ratio
Uniformly mixing, be then poured into copper standard flange, in atmosphere solidify after obtain 22.86mm × 10.16mm ×
2.52mm cuboid sample.
Carry out the measurement of electromagnetic parameter in 2-18GHz frequency ranges to it using waveguide method.
Specific testing result such as table 1.
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Complex dielectric permittivity | 0.03 | 0.01 | 0.08 | 1.21 |
| Complex permeability | 0.94 | 0.52 | 0.40 | 6.55 |
As shown in Table 1, the microwave absorption that prepared by the present invention has obvious absorption characteristic to microwave, and with the increasing of frequency
Add, microwave absorption capacity enhancing trend is notable, while preparation technology is simple, and cost is cheap, has a good application prospect.
Claims (7)
1. a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption, it is characterised in that concretely comprise the following steps：
（1）Take graphene oxide to add ultrasonic disperse in deionized water, add urea, be well mixed to obtain graphene dispersing solution；
（2）Cobalt chloride, frerrous chloride are taken, adds in hydrochloric acid and is well mixed, then under nitrogen atmosphere, be added dropwise to 1~2mL/min
In graphene dispersing solution, and be heated to 90~100 DEG C reaction 2~3h, stand 10~15h after filtration washing dry, obtain graphene/
Conjugate ferrite；
（3）Graphene/Conjugate ferrite, bismuth oxide, aluminum oxide, absolute ethyl alcohol are taken, is fitted into 20~24h of ball milling in ball mill, ball milling
20~30min of ultrasonic disperse in ethanol solution is transferred to after end, obtains codope Conjugate ferrite dispersion liquid；
（4）Tetraethyl orthosilicate is added dropwise into codope Conjugate ferrite dispersion liquid, ammoniacal liquor is added dropwise after well mixed, after stirring 8~10h
Filtration washing is dried, and obtains silicon coating-codoping Conjugate ferrite microwave absorption.
2. a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption as claimed in claim 1, its feature exist
In step（1）The graphene oxide and the mass ratio of deionized water are 1：250~1：1000, the amount of urea is oxidation
3.6~14.4 times of graphene quality.
3. a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption as claimed in claim 1, its feature exist
In step（2）The cobalt chloride, the mol ratio of frerrous chloride are 1：2, frerrous chloride dosage is the 2.5 of graphene oxide quality
~10 times.
4. a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption as claimed in claim 1, its feature exist
In step（3）Graphene/the Conjugate ferrite, bismuth oxide, aluminum oxide, the parts by weight of absolute ethyl alcohol are 10~20 parts of graphite
Alkene/Conjugate ferrite, 0.06~0.12 part of bismuth oxide, 0.12~0.24 part of aluminum oxide, 5~10 parts of absolute ethyl alcohols.
5. a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption as claimed in claim 1, its feature exist
In step（3）The mass fraction of the ethanol solution is 10%, and dosage is 10~40 times of graphene/Conjugate ferrite quality.
6. a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption as claimed in claim 1, its feature exist
In step（4）The dosage of the tetraethyl orthosilicate is the 25~100% of graphene/Conjugate ferrite quality.
7. a kind of preparation method of silicon coating-codoping Conjugate ferrite microwave absorption as claimed in claim 1, its feature exist
In step（4）The mass fraction of the ammoniacal liquor is 25%, and dosage is 1~4 times of graphene/Conjugate ferrite quality.
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Cited By (2)
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| CN109021919A (en) * | 2018-07-09 | 2018-12-18 | 中南大学 | A kind of preparation method and applications of graphene/cobalt nickel Mn ferrite nanocomposite |
| CN111257247A (en) * | 2019-11-22 | 2020-06-09 | 浙江省海洋水产研究所 | Method for measuring iron content in marine sediments |
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Cited By (4)
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Application publication date: 20180323 |