CN105111913B - Graphene/nanometer ferrite base aqueous electromagnetic shielding coating and preparation method thereof - Google Patents
Graphene/nanometer ferrite base aqueous electromagnetic shielding coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene/nanometer ferrite base aqueous electromagnetic shielding coating and preparation method thereof.Ferrite nanometer particle is carried on graphenic surface, prepare the graphene/ferrite nano composite for the good magnetic property of electric conductivity and nanometer ferrite for having graphene concurrently, then with aqueous film-forming resin and other auxiliary agents are compound prepares green environment protection water electromagnetic screen coating.The preparation method have it is simple to operate, practical, do not produce harmful substance, suitable different frequency can be produced as needed and the features such as the electromagnetic screen coating and shield effectiveness of occasion are good.Overcome the electromagnetic screen coating of prior art using single conductive or magnetic conduction substance as filler and there is the shortcomings of absorption band is narrow, shield effectiveness is poor.Graphene prepared by the present invention/ferrite base aqueous electromagnetic shielding coating has excellent electromagnetic shielding properties, therefore has good application prospect in electromagnetic screen coating field.
Description
Technical field
The invention belongs to electromagnetic wave screen paint field, and in particular to the aqueous electromagnetic shielding of graphene/nanometer ferrite base
Coating and preparation method thereof.
Background technology
Electronics, electric, communication and the life developed rapidly as people of information industry, work bring huge convenient same
When so that electromagenetic wave radiation pollution turn into after contaminated wastewater, exhaust emission, noxious waste pollution, noise pollution latter
New environmental pollution, not only causes severe jamming to people's periodic traffic equipment, computer and other electronic systems, and information is pacified
It is complete to cause serious threat, and immeasurable infringement is brought to health.Absorbing material is that a class can absorb, decay projection
To the electromagnetic wave on its surface, and convert it into the functional material that thermal energy consumption dissipates or made electromagnetic wave to be disappeared by interference.Using
Absorbing material prevents electromagenetic wave radiation pollution with environmental protection, ensured information safety and health, it has also become current international
The key subjects that upper effort is explored.In various absorbing materials, antiradar coatings are electromagnetic wave screen paint with its selection extensively,
Easy construction is flexible, practical and the features such as high cost performance and gains great popularity.
CN103205174A discloses a kind of electromagnetic masking electrically-conducting paint and preparation method thereof, and the coating is contained by adding
Magnesium dust assigns coating electric conductivity and electro-magnetic screen function.CN10389746A discloses a kind of high performance composite graphite alkene and led
The preparation method of electrocoating paint, the composite graphite alkene electrically-conducting paint is combined with graphene and inorganic coating and prepares electrically-conducting paint.
The electromagnetic screen coating of prior art almost using organic matter as solvent, is easily polluted to environment, and is had focused largely on single
Conductivity type coating.Single conductivity type coating haves the shortcomings that screening frequencies is narrow, shield effectiveness is relatively poor.Therefore exploitation has concurrently good
The compounded mix of good electric conductivity and magnetic is the key of High Performance Shielding coating.Graphene is former by individual layer hexagonal cellular carbon
Molecular cellular two dimensional crystal, it has high mechanical properties, excellent electric conductivity, high chemical stability the features such as, with it
He compares carbon material, and the special two-dimensional sheet structure of graphene and unique physicochemical properties cause it in absorbing material field
Application possess advantageous advantage.Ferrite wave-absorbing material is iron-series metal oxide or composite oxides, belongs to sub-
Ferrimagnet.Its absorbing property derives from ferromagnetism and dielectric properties, and its relative permeability and relative dielectric constant are in multiple
Number form formula, can produce dielectric loss can produce magnetic loss again, therefore with good absorbing property.Using graphene as conduction material
Material, can be ferritic by the excellent electric conductivity of graphene and nanostructured as the composite wave-suction material of permeability magnetic material using ferrite
Magnetic is combined, and coating can be made to be provided simultaneously with dielectric loss and magnetic loss, improves the absorbing property of single conductive filler.
The content of the invention
In view of this, in order to the electromagnetic screen coating shield effectiveness for solving the single conductive materials of prior art it is poor the problem of,
The invention discloses a kind of aqueous electromagnetic shielding coating using electric magnetoconductive composite material as filler and preparation method thereof, to have concurrently
Graphene and ferrite nano material are combined, prepared as filler by the composite wave-suction material of dielectric loss and magnetic loss
Have the graphene/nanometer ferrite composite wave-suction material of the good magnetic property of electric conductivity and nanometer ferrite of graphene concurrently, then with
Resin and other auxiliary agents are compound to prepare electromagnetic screen coating, then can make up graphene and only possess conduction loss and lacking without magnetic loss
Point.The impedance matching of electromagnetic absorption can be achieved, absorption frequency range is widened, improves the absorbing property of single conductive filler, so as to meet
Composite request of the practical application to electromagnetic shielding material " thin, light, wide, strong ".
The object of the present invention is achieved like this：Graphene/nanometer ferrite base aqueous electromagnetic shielding coating, by electromagnetic screen
Cover filler, aqueous film-forming resin, pure water, dispersant, coalescents composition；Its proportioning is by weight percentage：Electromagnetic shielding
Filler 10~55%, aqueous film-forming resin 30~70%, pure water 10~30%, dispersant 3~5%, coalescents 1~2%.
Described electromagnetic shielding filler is graphene/nanometer ferrite composite electromagnetic shield materials, it is characterised in that ferrite particle is born
It is loaded in flake graphite alkene surface.Ferrite formula is MFe2O4, wherein M is the one or more in Cu, Ni, Co, Mn, Zn, Fe；
Described aqueous film-forming resin is one kind in water-and acrylate, aqueous polyurethane, aqueous epoxy resins；Described dispersant
For one kind in cationic surfactant or anion surfactant or nonionic surface active agent；The coalescents
For alcohols, ester alcohol class, alcohol ethers or alcohol ether any one or two or more mix lipid.
The specific preparation process of the electromagnetic shielding waterborne paint is as follows：Graphene oxide is prepared by Hummers methods to disperse
Liquid；By the dissolving metal salts containing M and iron ion in water wiring solution-forming, the graphene oxide dispersion of certain volume is added, is surpassed
Sound is scattered 30 minutes；It is 11 with sodium hydroxide solution regulation pH value, is eventually adding Na2S2O3·5H2O, moves into reactor, seals,
It is placed in baking oven, 100 DEG C~220 DEG C stand reaction 1~48 hour；Graphene/nanometer ferrite is made after centrifuge washing to be combined
Electromagnetic shielding filler；Dispersant, pure water ultrasonic disperse are added after electromagnetic shielding filler grinding；Waterborne film-forming tree is added into again
In fat, film-forming resin grinding distribution in sand mill is added, makes its dispersed, that is, the aqueous electromagnetic shielding for obtaining the present invention is applied
Material.
Technical scheme is described below in detail：
A. the preparation of graphene oxide dispersion.Using natural flake graphite as raw material, oxidation stone is prepared using Hummers methods
Ink, is peeled off by graphite oxide ultrasound and prepares graphene oxide dispersion.Graphene oxide dispersion content is 0.1~20mg/mL；
B. the preparation of metal salt solution.Metal salt ultrasound containing M and iron ion is dissolved in graphene oxide dispersion,
Wherein M is Cu2+、Ni2+、Co2+、Mn2+、Zn2+、Fe2+In one or more；Acid ion in mixing salt solution is Cl-,
SO4 2-、NO3 -In one or more；
C. hydro-thermal reaction.Magnetic agitation autoclave is sealed, after 100~220 DEG C keep 1~48h, reaction to terminate
Room temperature is naturally cooled to, centrifuge washing obtains electromagnetic shielding filler；
D. electromagnetic shielding filler is pre-processed.Dispersant, pure water ultrasonic disperse are added toward electromagnetic shielding filler.
E. electromagnetic shielding filler after pretreatment added in aqueous film-forming resin, add coalescents and be placed in sand milling
Machine grinding makes its dispersed in 10 minutes, obtains the electromagnetic shielding waterborne paint of the present invention.
The beneficial effects of the invention are as follows：(1) coating, a side are prepared to load the graphene of ferrite nano material as filler
Face, the two-dimensional sheet structure of graphene makes it just be readily formed conductive network under a small amount of addition；On the other hand, graphene
The excellent ferritic magnetic of electric conductivity and nanostructured is combined, and coating can be made to be provided simultaneously with dielectric loss and magnetic loss, is realized
The impedance matching of electromagnetic absorption, widens absorption frequency range, improves the absorbing property of single conductive filler, so as to meet practical application pair
The composite request of electromagnetic shielding material " thin, light, wide, strong ".(2) existing electromagnetic screen coating preparation method is overcome generally to deposit
Cumbersome, the characteristics of Absorbing Materials and Modulatory character are poor.(3) present invention system is characterized using transmission electron microscope
The pattern of standby graphene/nanometer ferrite composite wave-suction material, present invention system is evaluated using the method for vector network analyzer
The absorbing property of standby graphene/nanometer ferrite base aqueous electromagnetic shielding coating, it is known that graphene/nanometer prepared by the present invention
Ferrite base aqueous electromagnetic shielding coating has excellent absorbing property, therefore has in electromagnetic screen coating field before application well
Scape.
The invention is further illustrated by the following examples, but the present invention is not restricted by the embodiments.It is all this
Within the spirit and principle of invention, any modification, equivalent substitution and improvements made etc. should be included in the protection model of the present invention
Within enclosing.
Embodiment
Embodiment one
The aqueous electromagnetic shielding coating formula is：
Electromagnetic shielding filler：10%
Water-and acrylate：70%
Pure water：16%
Dodecyl sodium sulfate：3%
The ester alcohol of coalescents 12：1%
It is prepared by electromagnetic shielding filler：It is stoichiometrically accurate to claim 0.27gFeCl3·6H2O(1mmol)、0.18gCoCl2·
6H2O (0.5mmol) is dissolved in 30mL water and is configured to solution, in the graphene oxide dispersion for the 15mg/mL for adding 2mL, ultrasound
30 minutes.It is 11 with sodium hydroxide solution (5M) regulation pH, is eventually adding reducing agent Na2S2O3·5H2O, loads reactor, close
Envelope, is placed in baking oven, and 150 DEG C are reacted 15 hours.Washing centrifugation directly obtains graphene/nanometer Conjugate ferrite composite.Fig. 1
For transmission electron microscope (Hitachi HT7700) photo of the present embodiment synthetic material, CoFe is can be seen that from the photo2O4Nanometer
Particle is evenly distributed on graphene sheet layer.Graphite prepared by the present invention is tested using X-ray diffractometer (Ultima IV)
The crystalline structure of alkene/nanometer ferrite composite wave-suction material, as shown in Figure 2.All diffraction maximums all with CoFe2O4Spinelle spreads out
Peak (JCPDS No.00-022-1086) is penetrated to match.And peak shape is sharp, illustrates CoFe2O4Crystal formation is complete, with good knot
Brilliant degree.
It is prepared by water-and acrylate electromagnetic screen coating：Graphene/nanometer ferrite obtained by preparation is added into dodecane
Base sodium sulfonate, pure water, carry out ultrasonic disperse, then are added into water-and acrylate, add coalescents, are placed in sand mill
The invention aqueous electromagnetic shielding coating is made in 10 minutes in grinding.Coating is cooled down 15 minutes, is applied on PVC substrates, normal temperature is done
Test shield effectiveness is 40dB (1.5G) after dry.
Embodiment two
The aqueous electromagnetic shielding coating formula is：
Electromagnetic shielding filler：10%
Aqueous polyurethane：68%
Pure water：16%
Lauryl sodium sulfate：5%
Coalescents Lauryl Alcohol ester：1%
It is prepared by electromagnetic shielding filler：Stoichiometrically precise 0.48gZn (NO3)2·6H2O (1.6mmol) and
1.31g Fe(NO3)3·9H2O (3.2mmol) is dissolved in 30mL water and is configured to solution, adds 2mL 20mg/mL graphite oxide
In alkene dispersion liquid, ultrasound 30 minutes.It is 11 with sodium hydroxide solution (5M) regulation pH, is eventually adding reducing agent Na2S2O3·
5H2O, loads reactor, and sealing is placed in baking oven, and 150 DEG C are reacted 15 hours.Washing centrifugation directly obtains graphene/nanometer copper
Ferrite composite material.
The preparation of aqueous polyurethane electromagnetic screen coating：Graphene/nanometer ferrite obtained by preparation is added into dodecane
Base sodium sulphate, pure water, carry out ultrasonic disperse, then are added into aqueous polyurethane, add coalescents, are placed in sand mill and grind
The invention aqueous electromagnetic shielding coating is made in 10 minutes in mill.Test shield effectiveness is 25dB (9.8G).
Embodiment three
The aqueous electromagnetic shielding coating formula is：
Electromagnetic shielding filler：20%
Aqueous epoxy resins：60%
Pure water：16%
OP-10：3%
Coalescents Dipropylene glycol mono-n-butyl Ether：1%
It is prepared by electromagnetic shielding filler：It is stoichiometrically accurate to claim 0.27gFeCl3·6H2O(1mmol)、0.06gNiCl2·
6H2O(0.25mmol)、0.09gCoCl2·6H2O (0.25mmol) is dissolved in 30mL water and is configured to solution, adds 2mL 15mg/
In mL graphene oxide dispersion, ultrasound 30 minutes.It is 11 with sodium hydroxide solution (5M) regulation pH, is eventually adding reducing agent
Na2S2O3·5H2O, loads reactor, and sealing is placed in baking oven, and 150 DEG C are reacted 24 hours.Washing centrifugation directly obtains graphite
Alkene/nanometer cobalt nickel ferrite composite.
The preparation of aqueous epoxy resins electromagnetic screen coating：Graphene/nanometer ferrite obtained by preparation is added into OP-
10th, pure water, carries out ultrasonic disperse, then is added into aqueous epoxy resins, adds coalescents, is placed in sand mill grinding 10
The invention aqueous electromagnetic shielding coating is made in minute.Test shield effectiveness is 30dB (3.5G).
Example IV
The aqueous electromagnetic shielding coating formula is：
Electromagnetic shielding filler：10%
Water-and acrylate：55%
Pure water：30%
Lauryl sodium sulfate：3%
Coalescents DAA：2%
It is prepared by electromagnetic shielding filler：Stoichiometrically precise 0.33g CuSO4(1.3mmol) and 1.05g Fe2
(SO4)3(2.6mmol) is dissolved in 30mL water and is configured to solution, in the graphene oxide dispersion for the 20mg/mL for adding 2mL, surpasses
Sound 30 minutes.It is 11 with sodium hydroxide solution (5M) regulation pH, is eventually adding reducing agent Na2S2O3·5H2O, loads reactor,
Sealing, is placed in baking oven, and 150 DEG C are reacted 48 hours.Washing centrifugation directly obtains graphene/nanometer Zn ferrite composite.
The preparation of water-and acrylate electromagnetic screen coating：Graphene/nanometer ferrite obtained by preparation is added 12
Sodium alkyl sulfate, pure water, carry out ultrasonic disperse, then are added into water-and acrylate, add coalescents, are placed in sand milling
Machine grinds 10 minutes and the invention aqueous electromagnetic shielding coating is made.Test shield effectiveness is 25dB (4.5G).
Embodiment five
The aqueous electromagnetic shielding coating formula is：
Electromagnetic shielding filler：55%
Aqueous polyurethane：30%
Pure water：10%
Neopelex：4%
Coalescents DAA：1%
It is prepared by electromagnetic shielding filler：It is stoichiometrically accurate to claim 0.27gFeCl3·6H2O(1mmol)、0.12gNiCl2·
6H2O (0.5mmol) is dissolved in 30mL water and is configured to solution, in the graphene oxide dispersion for the 15mg/mL for adding 2mL, ultrasound
30 minutes.It is 11 with sodium hydroxide solution (5M) regulation pH, is eventually adding reducing agent Na2S2O3·5H2O, loads reactor, close
Envelope, is placed in baking oven, and 100 DEG C are reacted 12 hours.Washing centrifugation directly obtains graphene/nanometer Ni ferrite composite.
The preparation of aqueous polyurethane electromagnetic screen coating：Graphene/nanometer ferrite obtained by preparation is added into dodecane
Base benzene sulfonic acid sodium salt, pure water, carry out ultrasonic disperse, then are added into aqueous polyurethane, add coalescents, are placed in sand mill
The invention aqueous electromagnetic shielding coating is made in 10 minutes in grinding.Test shield effectiveness is 45dB (1.5G).
Brief description of the drawings:
Fig. 1 is the transmission electron microscope photo of graphene/nanometer ferrite composite material；
Fig. 2 is the XRD spectrum of graphene/nanometer ferrite composite material.
Claims (1)
1. a kind of preparation method using graphene/nanometer ferrite as the aqueous electromagnetic shielding coating of filler, it is characterised in that:Should
Aqueous electromagnetic shielding coating formula is：
Electromagnetic shielding filler：10%
Water-and acrylate：70%
Pure water：16%
Dodecyl sodium sulfate：3%
The ester alcohol of coalescents 12：1%；
It is prepared by electromagnetic shielding filler：It is stoichiometrically accurate to claim 0.27gFeCl3·6H2O、0.18gCoCl2·6H2O is dissolved in
30mL water is configured to solution, in the graphene oxide dispersion for the 15mg/mL for adding 2mL, ultrasound 30 minutes；It is molten with sodium hydroxide
Liquid regulation pH is 11, is eventually adding reducing agent Na2S2O3·5H2O, loads reactor, and sealing is placed in baking oven, 150 DEG C of reactions
15 hours；Washing centrifugation directly obtains graphene/nanometer Conjugate ferrite composite；
It is prepared by aqueous electromagnetic shielding coating：Graphene/nanometer Conjugate ferrite composite obtained by preparation is added into dodecyl
Sodium sulfonate, pure water, carry out ultrasonic disperse, then are added into water-and acrylate, add coalescents, are placed in sand mill and grind
Aqueous electromagnetic shielding coating is made in 10 minutes in mill；Coating is cooled down 15 minutes, is applied on PVC substrates, air drying.
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