CN107896476A - A kind of magnetic nano-particle microwave absorbing material and preparation method thereof - Google Patents
A kind of magnetic nano-particle microwave absorbing material and preparation method thereof Download PDFInfo
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- CN107896476A CN107896476A CN201711001760.4A CN201711001760A CN107896476A CN 107896476 A CN107896476 A CN 107896476A CN 201711001760 A CN201711001760 A CN 201711001760A CN 107896476 A CN107896476 A CN 107896476A
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Abstract
The invention discloses a kind of magnetic nano-particle microwave absorbing material and preparation method thereof, by molybdenum disilicide, silica, sodium carboxymethylcellulose, iron chloride, chitosan, the raw materials such as citric acid are made, composite wave-suction material of the present invention had not only had ferrimagnetism but also had had dielectric properties, its relative permeability and relative conductivity are in plural form, dielectric loss and can be produced and produce magnetic hystersis loss, absorbing property is good, it is narrow to overcome traditional absorbing material frequency band, efficiency is low, the shortcomings of density is big, preparation method is relatively easy simultaneously, it is suitable for daily household electrical appliances and factory, the surface microwave absorbing coating of research equipment uses.
Description
Technical field
The present invention relates to absorbing material technical field, more particularly to a kind of magnetic nano-particle microwave absorbing material and its system
Preparation Method.
Background technology
In today of development in science and technology, mobile phone, computer and all kinds of household electrical appliances are also brought not while bringing people and facilitating
Hold the hazards of electromagnetic radiation ignored, in order to reduce its radiation to human body, especially head as far as possible, except reducing radiant power
And contact of the reduction with human body when ensureing to use, it is also contemplated that other safeguard procedures.
Industry, science and Medical Devices can also produce substantial amounts of electromagnetic radiation in the course of the work, if dealt with improperly, no
The working environment of itself can only be caused damage, while the equipment of surrounding can also be interfered, so as to be brought to scientific research, production
High resistance, the electromagnetic radiation that these equipment are sent in addition also can bring harm to the health of operating personnel.Therefore, to work
It is very necessary that industry, science and Medical Devices carry out electromagnetic radiation protection.
Magnetic nano-particle is as a kind of new material developed in recent years, not only with nano effect, i.e. surface
Effect, small-size effect, macro quanta tunnel effect and bulk effect, also with magnetic property, such as superparamagnetism and high magnetization
The characteristics such as rate.Its application develops into high-technology field from traditional technical field, is expanded to from simple magnetics scope
The interdisciplinary field related to magnetics.Among these ferroferric oxide magnetic nano-particles on the one hand because its have can be with biology
The special functional group of active material reaction, can be as the carrier of bioactive substance, on the other hand again because it has superparamagnetic
Property, it in the presence of externally-applied magnetic field, can quickly, simply separate, make it in wastewater treatment, exhaust-gas treatment, soil remediation, microwave
The research in the fields such as absorption becomes increasingly active, and shows preferable application prospect.
Ferrite nano absorbing material, which has, among these absorbs the advantages of strong, frequency band is wider and cost is low, but its have compared with
Big density and relatively low Curie temperature and poor high temperature stability etc., in high temperature environments with their suction ripple in high band range
Performance comparision is poor, limits its application in specific environment.Additionally due to the size of nano-particle is very small, have very high
Surface energy, it is a kind of thermodynamic unstable system, is easily agglomerated into larger particle, and because nanoparticle surface is with many
Chemical bond, can have a very active chemical property, due to magnetic dipole gravitation between particle, easily reunite, easily aggregate into two
Secondary particle, be not easy to disperse, thus compared in general nano-particle for, the surface of nano-particle is modified and just very must
Will.
The content of the invention
A kind of the defects of the object of the invention is exactly to make up prior art, there is provided magnetic nano-particle microwave absorbing material
And preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of magnetic nano-particle microwave absorbing material, is prepared by the following method:
(1)By molybdenum disilicide, silica, sodium carboxymethylcellulose in mass ratio(6-7):(15-18):(1-2)Add after mixing
Enter in water, grind 5-6 hours, obtain mixed slurry, it is dried to moisture evaporating completely at 90-100 DEG C, obtains mixed powder;
(2)Iron chloride is pressed into solid-to-liquid ratio 1:(28-32)G/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then thereto
Anhydrous sodium acetate and polyethylene glycol are added, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1:(2.5-2.7):
(0.7-0.8), 50-55 DEG C is warming up to, is stirred continuously to uniform mixed liquor is formed, ultrasonic disperse is uniformly sent into reactor afterwards,
200-220 DEG C is warming up to, taking-up is cooled to room temperature after reacting 5-6 hours, and alternately cleaning removes impurity with ethanol and clear water, will
Gained solid is dried, and obtains SPIO;
(3)Step 2 gained ferriferrous oxide nano-particle is dispersed in 20-25% ethanol solutions, then adds shell thereto
Glycan and citric acid, mixed liquor is transferred in agitator, connection nitrogen protection, is warming up to 35-40 DEG C and with 800-1000 revs/min
30-40 minutes are stirred, products therefrom ethanol and clear water are alternately cleaned after stirring, until pH is 7, are re-fed into drying box
In dried, it is standby that chitosan-citric acid duplex surface modification magnetic ferroferric oxide nano-particles are obtained after grinding;
(4)By step 1 gained mixed powder and step 3 gained nano-particle in mass ratio(1-1.2):1 mixing after add go from
Sub- water stirs 4-6 hours, after the completion of be placed at 90-100 DEG C and dried to moisture evaporating completely again.It is standby to obtain powder;
(5)Step 4 gained powder is heated under 20-50MPa pressure, that is, obtains microwave absorbing material of the present invention.
Molybdenum disilicide, silica, the mass ratio of sodium carboxymethylcellulose are 6 in the step 1:18:1.
Ultrasound condition is that 10-12 minutes are ultrasonically treated under 35-38kHz in the step 2.
Ferriferrous oxide nano-particle, chitosan, the mass ratio of citric acid are in the step 3(5-6):(1-1.2):
(2-2.5).
Temperature is first heated to 600-700 DEG C when heating in the step 5, is kept for 80-100 minutes, is further continued for adding
Heat is kept for 30-40 minutes to 1000-1200 DEG C, stops heating and being down to naturally room temperature afterwards.
It is an advantage of the invention that:
The present invention is compound using molybdenum disilicide, silica, ferriferrous oxide nano-particle progress, by it chemically and physically
Compatibility, improve its continuation and elevated temperature strength as absorbing material, ferriferrous oxide nano-particle is gathered with shell among these
Sugar and citric acid is compound carries out surface modification to it, has been utilized respectively the electronegative polar end of citric acid by Coulomb force and four oxygen
Change three-iron institute it is positively charged attract each other and chitosan in functional group and its surface form chemical bonds so as to four oxygen
Change three-iron particle surface locally to coat, improve its inoxidizability, biocompatibility and dispersion stabilization in use, institute
The composite wave-suction material obtained has not only had ferrimagnetism but also had had dielectric properties, and its relative permeability and relative conductivity are in plural shape
Formula, can produce dielectric loss and can produce magnetic hystersis loss, absorbing property is good, overcome traditional absorbing material frequency band it is narrow, effect
The shortcomings of rate is low, density is big, while preparation method is relatively easy, is suitable for daily household electrical appliances and factory, the surface of research equipment inhale
Ripple coating uses.
Embodiment
A kind of magnetic nano-particle microwave absorbing material, is prepared by the following method:
(1)By molybdenum disilicide, silica, sodium carboxymethylcellulose in mass ratio 6:18:It is added to the water after 1 mixing, grinding 5 is small
When, mixed slurry is obtained, it is dried to moisture evaporating completely at 90 DEG C, obtains mixed powder;
(2)Iron chloride is pressed into solid-to-liquid ratio 1:30g/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then add nothing thereto
Water sodium acetate and polyethylene glycol, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1:2.5:0.8, it is warming up to 50
DEG C, it is stirred continuously to uniform mixed liquor is formed, is ultrasonically treated under 35kHz 10 minutes and is sent into after being uniformly dispersed in reactor, risen
Temperature to 200 DEG C, after 5 hours take out and be cooled to room temperature by reaction, and alternately cleaning removes impurity with ethanol and clear water, by gained solid
Dry, obtain SPIO;
(3)Step 2 gained ferriferrous oxide nano-particle is dispersed in 20% ethanol solution, then adds shell thereto and gathers
Sugar and citric acid, wherein ferriferrous oxide nano-particle, chitosan, the mass ratio of citric acid are 6:1:2.4, mixed liquor is transferred to
In agitator, connection nitrogen protection, it is warming up to 35 DEG C and is stirred 30 minutes with 800 revs/min, use products therefrom after stirring
Ethanol and clear water alternately clean, until pH is 7, is re-fed into drying box and is dried, chitosan citrate is obtained after grinding and is answered
It is standby to close surface modified magnetic ferriferrous oxide nano-particle;
(4)By step 1 gained mixed powder and step 3 gained nano-particle in mass ratio 1.2:Deionized water is added after 1 mixing
Stirring 4 hours, after the completion of be placed at 90 DEG C and dried to moisture evaporating completely again.It is standby to obtain powder;
(5)Step 4 gained powder is heated under 35MPa pressure, temperature is first heated to 600 DEG C, is kept for 80 points
Clock, it is further continued for being heated to 1000 DEG C, is kept for 30 minutes, stops heating afterwards and be down to room temperature naturally, that is, obtain microwave of the present invention
Absorbing material.
Claims (5)
1. a kind of magnetic nano-particle microwave absorbing material, it is characterised in that be prepared by the following method:
(1)By molybdenum disilicide, silica, sodium carboxymethylcellulose in mass ratio(6-7):(15-18):(1-2)Add after mixing
Enter in water, grind 5-6 hours, obtain mixed slurry, it is dried to moisture evaporating completely at 90-100 DEG C, obtains mixed powder;
(2)Iron chloride is pressed into solid-to-liquid ratio 1:(28-32)G/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then thereto
Anhydrous sodium acetate and polyethylene glycol are added, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1:(2.5-2.7):
(0.7-0.8), 50-55 DEG C is warming up to, is stirred continuously to uniform mixed liquor is formed, ultrasonic disperse is uniformly sent into reactor afterwards,
200-220 DEG C is warming up to, taking-up is cooled to room temperature after reacting 5-6 hours, and alternately cleaning removes impurity with ethanol and clear water, will
Gained solid is dried, and obtains SPIO;
(3)Step 2 gained ferriferrous oxide nano-particle is dispersed in 20-25% ethanol solutions, then adds shell thereto
Glycan and citric acid, mixed liquor is transferred in agitator, connection nitrogen protection, is warming up to 35-40 DEG C and with 800-1000 revs/min
30-40 minutes are stirred, products therefrom ethanol and clear water are alternately cleaned after stirring, until pH is 7, are re-fed into drying box
In dried, it is standby that chitosan-citric acid duplex surface modification magnetic ferroferric oxide nano-particles are obtained after grinding;
(4)By step 1 gained mixed powder and step 3 gained nano-particle in mass ratio(1-1.2):1 mixing after add go from
Sub- water stirs 4-6 hours, after the completion of be placed at 90-100 DEG C and dried to moisture evaporating completely again, it is standby to obtain powder;
(5)Step 4 gained powder is heated under 20-50MPa pressure, that is, obtains microwave absorbing material of the present invention.
2. the preparation method of magnetic nano-particle microwave absorbing material according to claim 1, it is characterised in that the step
Molybdenum disilicide, silica, the mass ratio of sodium carboxymethylcellulose are 6 in rapid 1:18:1.
3. the preparation method of magnetic nano-particle microwave absorbing material according to claim 1, it is characterised in that the step
Ultrasound condition is that 10-12 minutes are ultrasonically treated under 35-38kHz in rapid 2.
4. the preparation method of magnetic nano-particle microwave absorbing material according to claim 1, it is characterised in that the step
Ferriferrous oxide nano-particle, chitosan, the mass ratio of citric acid are in rapid 3(5-6):(1-1.2):(2-2.5).
5. the preparation method of magnetic nano-particle microwave absorbing material according to claim 1, it is characterised in that the step
Temperature is first heated to 600-700 DEG C when heating in rapid 5, is kept for 80-100 minutes, is further continued for being heated to 1000-1200
DEG C, kept for 30-40 minutes, stop heating and being down to naturally room temperature afterwards.
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Cited By (1)
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CN110021461A (en) * | 2019-03-06 | 2019-07-16 | 苏州蓝沛光电科技有限公司 | The production method of transparent conductive film structure |
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CN110021461A (en) * | 2019-03-06 | 2019-07-16 | 苏州蓝沛光电科技有限公司 | The production method of transparent conductive film structure |
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Application publication date: 20180410 |