CN105111913A - Graphene/nano ferrite based water electromagnetic shielding paint and preparation method thereof - Google Patents

Graphene/nano ferrite based water electromagnetic shielding paint and preparation method thereof Download PDF

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Publication number
CN105111913A
CN105111913A CN201510644047.6A CN201510644047A CN105111913A CN 105111913 A CN105111913 A CN 105111913A CN 201510644047 A CN201510644047 A CN 201510644047A CN 105111913 A CN105111913 A CN 105111913A
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electromagnetic shielding
graphene
aqueous
ferrite
preparation
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CN105111913B (en
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赵芸
王燕枫
矫庆泽
黎汉生
吴芹
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Beijing Institute of Technology BIT
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Beijing Institute of Technology BIT
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Abstract

The invention discloses a graphene/nano ferrite based water electromagnetic shielding paint and a preparation method thereof. Ferrite nanoparticles are loaded on the surface of graphene to prepare a graphene/ferrite nanocomposite with the electrical conductivity of the graphene and the good magnetic property of the nano ferrite, and then the nanocomposite is combined with a water film-forming resin and other auxiliaries to prepare the green and environment-friendly water electromagnetic shielding paint. The preparation method has the characteristics of being simple to operate, high in practicability, free of hazardous substance, capable of making electromagnetic shielding paints suitable for different frequencies and occasions, good in shielding effect, and the like; the prepared graphene/nano ferrite based water electromagnetic shielding paint has excellent electromagnetic shielding performance, and therefore has good application prospect in the field of electromagnetic shielding paints.

Description

Graphene/nanometer ferrite base aqueous electromagnetic shielding coating and preparation method thereof
Technical field
The invention belongs to electromagnetic wave screen paint field, be specifically related to graphene/nanometer ferrite base aqueous electromagnetic shielding coating and preparation method thereof.
Background technology
Electronics, electrically, the develop rapidly of communication and information industry is the life of people, work bring huge simultaneously easily, electromagenetic wave radiation is polluted and becomes a kind of new environmental pollution after contaminated wastewater, exhaust emission, noxious waste pollution, sound pollution, not only severe jamming is caused to people's periodic traffic equipment, computer and other electronic system, serious threat is caused to information security, and immeasurable infringement is brought to HUMAN HEALTH.Absorbing material is that a class can absorb, decaying projects the hertzian wave on its surface, and converts it into the functional materials that thermal energy consumption dissipates or make hertzian wave to disappear because of interference.Adopt absorbing material to prevent electromagenetic wave radiation from polluting with protection of the environment, ensuring information safety and HUMAN HEALTH, become current key subjects of making great efforts to explore in the world.In various absorbing material, antiradar coatings and electromagnetic wave screen paint are extensive with its selection, easy construction is flexible, practical and cost performance high and gaining great popularity.
CN103205174A discloses a kind of electromagnetic masking electrically conducting coating and preparation method thereof, and this coating gives coating electroconductibility and electro-magnetic screen function by adding containing magnesium dust.CN10389746A discloses a kind of preparation method of high performance composite graphite alkene electrically conducting coating, and this composite graphite alkene electrically conducting coating combines with Graphene and inorganic paint and prepares electrically conducting coating.The electromagnetic screen coating of prior art, almost using organism as solvent, easily to environment, and concentrates on single conductivity type coating mostly.There is the shortcoming that screening frequencies is narrow, effectiveness of shielding is relatively poor in single conductivity type coating.Therefore exploitation has the key that the compounded mix of satisfactory electrical conductivity and magnetic is High Performance Shielding coating concurrently.The cellular two dimensional crystal that Graphene is made up of individual layer hexagonal cellular carbon atom, it has high mechanical strength, the excellent feature such as electroconductibility, high chemical stability, compared with other carbon materials, the two-dimensional sheet structure that Graphene is special and unique physicochemical property make it possess advantageous advantage in the application in absorbing material field.Ferrite wave-absorbing material is iron-series metal oxide or composite oxides, belongs to ferrimagnetic material.Its absorbing property derives from ferromegnetism and dielectric properties, and its relative magnetic permeability and relative permittivity, all in plural form, can produce dielectric loss and can produce magnetic loss again, therefore have good absorbing property.Be electro-conductive material with Graphene, be that the electroconductibility of Graphene excellence and the ferritic Magnetic Phase of nanostructure can combine by the composite wave-suction material of magnetically permeable material with ferrite, coating can be made simultaneously to possess dielectric loss and magnetic loss, improve the absorbing property of single conductive filler material.
Summary of the invention
In view of this, in order to solve the problem of the electromagnetic screen coating effectiveness of shielding difference of the single conducting material of prior art, the invention discloses a kind of take electric magnetoconductive composite material as aqueous electromagnetic shielding coating of filler and preparation method thereof, to have the composite wave-suction material of dielectric loss and magnetic loss concurrently as filler, Graphene and ferrite nano material are carried out compound, prepare the graphene/nanometer ferrite composite wave-suction material of electroconductibility and the good magnetic property of nanometer ferrite having Graphene concurrently, electromagnetic screen coating is prepared again with resin and other auxiliary agent compound, then can make up Graphene and only possess conduction loss and without the shortcoming of magnetic loss.The impedance matching of electromagnetic absorption can be realized, widen absorption frequency range, improve the absorbing property of single conductive filler material, thus meet the composite request of 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, is made up of electromagnetic shielding filler, aqueous film-forming resin, pure water, dispersion agent, film coalescence aid; Its proportioning is by weight percentage: electromagnetic shielding filler 10 ~ 55%, aqueous film-forming resin 30 ~ 70%, pure water 10 ~ 30%, dispersion agent 3 ~ 5%, film coalescence aid 1 ~ 2%.Described electromagnetic shielding filler is graphene/nanometer ferrite composite electromagnetic shield materials, it is characterized in that, ferrite paricles particle loading is on flake graphite alkene surface.Ferrite general formula is MFe 2o 4, wherein M is one or more in Cu, Ni, Co, Mn, Zn, Fe; Described aqueous film-forming resin is the one in water-and acrylate, aqueous polyurethane, aqueous epoxy resins; Described dispersion agent is the one in cats product or anion surfactant or nonionic surface active agent; Described film coalescence aid is alcohols, ester alcohols, alcohol ethers or alcohol ether any one or two or morely mix lipid.
The concrete preparation process of this electromagnetic shielding waterborne paint is as follows: by Hummers legal system for graphene oxide dispersion; By the dissolving metal salts containing M and iron ion in water wiring solution-forming, add the graphene oxide dispersion of certain volume, ultrasonic disperse 30 minutes; Be 11 by sodium hydroxide solution adjust ph, finally add Na 2s 2o 35H 2o, moves into reactor, and sealing, is placed in baking oven, 100 DEG C ~ 220 DEG C standing and reacting 1 ~ 48 hour; Obtained graphene/nanometer ferrite composite electromagnetic screen filler after centrifuge washing; Dispersion agent, pure water ultrasonic disperse is added after electromagnetic shielding filler grinding; Added again in aqueous film-forming resin, add film-forming resin grinding distribution in sand mill, make it dispersed, namely obtain aqueous electromagnetic shielding coating of the present invention.
Technical scheme of the present invention is described below in detail:
A. the preparation of graphene oxide dispersion.Take natural flake graphite as raw material, adopt Hummers legal system for graphite oxide, prepare graphene oxide dispersion by the ultrasonic stripping of graphite oxide.Graphene oxide dispersion content is 0.1 ~ 20mg/mL;
B. the preparation of metal salt solution.Be dissolved in graphene oxide dispersion by ultrasonic for the metal-salt containing M and iron ion, wherein M is Cu 2+, Ni 2+, Co 2+, Mn 2+, Zn 2+, Fe 2+in one or more; Acid ion in mixing salt solution is Cl -, SO 4 2-, NO 3 -in one or more;
C. hydro-thermal reaction.Sealed by magnetic agitation autoclave, keep 1 ~ 48h at 100 ~ 220 DEG C, naturally cool to room temperature after reaction terminates, centrifuge washing obtains electromagnetic shielding filler;
D. electromagnetic shielding filler pre-treatment.Dispersion agent, pure water ultrasonic disperse is added toward electromagnetic shielding filler.
E. electromagnetic shielding filler after pretreatment to be added in aqueous film-forming resin, add film coalescence aid again and be placed in sand mill and grind and make it dispersed in 10 minutes, obtain electromagnetic shielding waterborne paint of the present invention.
The invention has the beneficial effects as follows: (1), with the Graphene of load iron oxysome nano material for coating prepared by filler, on the one hand, the two-dimensional sheet structure of Graphene makes it just be easy to form conductive network under a small amount of addition; On the other hand, the electroconductibility of Graphene excellence and the ferritic Magnetic Phase of nanostructure combine, coating can be made to possess dielectric loss and magnetic loss simultaneously, realize the impedance matching of electromagnetic absorption, widen absorption frequency range, improve the absorbing property of single conductive filler material, thus meet the composite request of practical application to electromagnetic shielding material " thin, light, wide, strong ".(2) the ubiquitous complex operation of existing electromagnetic screen coating preparation method is overcome, the feature of Absorbing Materials and Modulatory character difference.(3) transmission electron microscope is adopted to characterize the pattern of graphene/nanometer ferrite composite wave-suction material prepared by the present invention, the absorbing property of the graphene/nanometer ferrite base aqueous electromagnetic shielding coating adopting method evaluation the present invention of vector network analyzer to prepare, graphene/nanometer ferrite base aqueous electromagnetic shielding coating prepared by known the present invention has excellent absorbing property, therefore has good application prospect in electromagnetic screen coating field.
The invention is further illustrated by the following examples, but the present invention is not by the restriction of these embodiments.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Embodiment
Embodiment one
This aqueous electromagnetic shielding coating formula is:
Electromagnetic shielding filler: 10%
Water-and acrylate: 70%
Pure water: 16%
Sodium laurylsulfonate: 3%
Film coalescence aid ten diester alcohol: 1%
Prepared by electromagnetic shielding filler: stoichiometrically accurately claim 0.27gFeCl 36H 2o (1mmol), 0.18gCoCl 26H 2o (0.5mmol) is dissolved in 30mL water and is mixed with solution, adds in the graphene oxide dispersion of the 15mg/mL of 2mL, ultrasonic 30 minutes.Regulate pH to be 11 with sodium hydroxide solution (5M), finally add reductive agent Na 2s 2o 35H 2o, loads reactor, and sealing, is placed in baking oven, and 150 DEG C are reacted 15 hours.Wash and centrifugally directly obtain graphene/nanometer vectolite matrix material.Fig. 1 is transmission electron microscope (HitachiHT7700) photo of the present embodiment synthetic materials, can find out CoFe from this photo 2o 4nano particle is evenly distributed on graphene sheet layer.X-ray diffractometer (UltimaIV) is adopted to test the crystalline structure of graphene/nanometer ferrite composite wave-suction material prepared by the present invention, as shown in Figure 2.All diffraction peaks all with CoFe 2o 4(JCPDSNo.00-022-1086) matches at spinel diffraction peak.And peak shape is sharp-pointed, and CoFe is described 2o 4crystal formation is complete, has good degree of crystallinity.
Prepared by water-and acrylate electromagnetic screen coating: the graphene/nanometer ferrite preparing gained is added sodium laurylsulfonate, pure water, carry out ultrasonic disperse, added again in water-and acrylate, add film coalescence aid, be placed in sand mill and grind 10 minutes i.e. these invention aqueous electromagnetic shielding coatings obtained.Coating is cooled 15 minutes, be applied on PVC substrate, testing effectiveness of shielding after Air drying is 40dB (1.5G).
Embodiment two
This aqueous electromagnetic shielding coating formula is:
Electromagnetic shielding filler: 10%
Aqueous polyurethane: 68%
Pure water: 16%
Sodium lauryl sulphate: 5%
Film coalescence aid Lauryl Alcohol ester: 1%
Prepared by electromagnetic shielding filler: stoichiometrically precise 0.48gZn (NO 3) 26H 2o (1.6mmol) and 1.31gFe (NO 3) 39H 2o (3.2mmol) is dissolved in 30mL water and is mixed with solution, adds in the graphene oxide dispersion of the 20mg/mL of 2mL, ultrasonic 30 minutes.Regulate pH to be 11 with sodium hydroxide solution (5M), finally add reductive agent Na 2s 2o 35H 2o, loads reactor, and sealing, is placed in baking oven, and 150 DEG C are reacted 15 hours.Wash and centrifugally directly obtain graphene/nanometer copper ferrite composite material.
The preparation of aqueous polyurethane electromagnetic screen coating: the graphene/nanometer ferrite preparing gained is added sodium lauryl sulphate, pure water, carry out ultrasonic disperse, added again in aqueous polyurethane, add film coalescence aid, be placed in sand mill and grind 10 minutes i.e. these invention aqueous electromagnetic shielding coatings obtained.Test effectiveness of shielding is 25dB (9.8G).
Embodiment three
This aqueous electromagnetic shielding coating formula is:
Electromagnetic shielding filler: 20%
Aqueous epoxy resins: 60%
Pure water: 16%
OP-10：3％
Film coalescence aid Dipropylene glycol mono-n-butyl Ether: 1%
Prepared by electromagnetic shielding filler: stoichiometrically accurately claim 0.27gFeCl 36H 2o (1mmol), 0.06gNiCl 26H 2o (0.25mmol), 0.09gCoCl 26H 2o (0.25mmol) is dissolved in 30mL water and is mixed with solution, adds in the graphene oxide dispersion of the 15mg/mL of 2mL, ultrasonic 30 minutes.Regulate pH to be 11 with sodium hydroxide solution (5M), finally add reductive agent Na 2s 2o 35H 2o, loads reactor, and sealing, is placed in baking oven, and 150 DEG C are reacted 24 hours.Wash and centrifugally directly obtain graphene/nanometer cobalt nickel ferrite matrix material.
The preparation of aqueous epoxy resins electromagnetic screen coating: the graphene/nanometer ferrite preparing gained is added OP-10, pure water, carry out ultrasonic disperse, added again in aqueous epoxy resins, add film coalescence aid, be placed in sand mill and grind 10 minutes i.e. these invention aqueous electromagnetic shielding coatings obtained.Test effectiveness of shielding is 30dB (3.5G).
Embodiment four
This aqueous electromagnetic shielding coating formula is:
Electromagnetic shielding filler: 10%
Water-and acrylate: 55%
Pure water: 30%
Sodium lauryl sulphate: 3%
Film coalescence aid diacetone alcohol: 2%
Prepared by electromagnetic shielding filler: stoichiometrically precise 0.33gCuSO 4(1.3mmol) and 1.05gFe 2(SO 4) 3(2.6mmol) be dissolved in 30mL water and be mixed with solution, add in the graphene oxide dispersion of the 20mg/mL of 2mL, ultrasonic 30 minutes.Regulate pH to be 11 with sodium hydroxide solution (5M), finally add reductive agent Na 2s 2o 35H 2o, loads reactor, and sealing, is placed in baking oven, and 150 DEG C are reacted 48 hours.Wash and centrifugally directly obtain graphene/nanometer Zn ferrite matrix material.
The preparation of water-and acrylate electromagnetic screen coating: the graphene/nanometer ferrite preparing gained is added sodium lauryl sulphate, pure water, carry out ultrasonic disperse, added again in water-and acrylate, add film coalescence aid, be placed in sand mill and grind 10 minutes i.e. these invention aqueous electromagnetic shielding coatings obtained.Test effectiveness of shielding is 25dB (4.5G).
Embodiment five
This aqueous electromagnetic shielding coating formula is:
Electromagnetic shielding filler: 55%
Aqueous polyurethane: 30%
Pure water: 10%
Sodium dodecylbenzene sulfonate: 4%
Film coalescence aid diacetone alcohol: 1%
Prepared by electromagnetic shielding filler: stoichiometrically accurately claim 0.27gFeCl 36H 2o (1mmol), 0.12gNiCl 26H 2o (0.5mmol) is dissolved in 30mL water and is mixed with solution, adds in the graphene oxide dispersion of the 15mg/mL of 2mL, ultrasonic 30 minutes.Regulate pH to be 11 with sodium hydroxide solution (5M), finally add reductive agent Na 2s 2o 35H 2o, loads reactor, and sealing, is placed in baking oven, and 100 DEG C are reacted 12 hours.Wash and centrifugally directly obtain graphene/nanometer Ni ferrite matrix material.
The preparation of aqueous polyurethane electromagnetic screen coating: the graphene/nanometer ferrite preparing gained is added Sodium dodecylbenzene sulfonate, pure water, carry out ultrasonic disperse, added again in aqueous polyurethane, add film coalescence aid, be placed in sand mill and grind 10 minutes i.e. these invention aqueous electromagnetic shielding coatings obtained.Test effectiveness of shielding is 45dB (1.5G).
Accompanying drawing illustrates:
Fig. 1 is the transmission electron microscope photo of graphene/nanometer ferrite composite material;
Fig. 2 is the XRD figure spectrum of graphene/nanometer ferrite composite material.

Claims (6)

1. graphene/nanometer ferrite base aqueous electromagnetic shielding coating and preparation method thereof, is characterized in that: be made up of electromagnetic shielding filler, aqueous film-forming resin, pure water, dispersion agent, film coalescence aid; Its proportioning is by weight percentage: electromagnetic shielding filler 10 ~ 55%, aqueous film-forming resin 30 ~ 70%, pure water 10 ~ 30%, dispersion agent 3 ~ 5%, film coalescence aid 1% ~ 2%.
2. electromagnetic shielding filler as claimed in claim 1 is Graphene/ferrite nano matrix material, and it is characterized in that, general formula is MFe 2o 4ferrite nanometer particle load flake graphite alkene surface, wherein M is one or more in Cu, Ni, Co, Mn, Zn, Fe.
3. a kind of aqueous electromagnetic shielding coating as claimed in claim 1, is characterized in that: aqueous film-forming resin is the one in water-and acrylate, aqueous polyurethane, aqueous epoxy resins.
4. a kind of aqueous electromagnetic shielding coating as claimed in claim 1, is characterized in that: dispersion agent is the one of cats product or anion surfactant or nonionic surface active agent.
5. a kind of aqueous electromagnetic shielding coating as claimed in claim 1, is characterized in that, above-mentioned film coalescence aid is alcohols, ester alcohols, ester ethers or alcohol ether-ether class any one or two or morely to mix.
6. the preparation method of an aqueous electromagnetic shielding coating, it is characterized in that: its preparation process is: by the dissolving metal salts containing M and iron ion in water wiring solution-forming, add certain volume through the standby graphene oxide dispersion of Hummers legal system, ultrasonic disperse 30 minutes; Be 11 by sodium hydroxide adjust ph, finally add Na 2s 2o 35H 2o, loads reactor, and sealing, is placed in baking oven, 100 DEG C ~ 220 DEG C standing and reacting 1 ~ 48 hour; The rear obtained Graphene/ferrite composite electromagnetic screen filler of centrifugal, washing; Add dispersion agent, pure water ultrasonic disperse obtains graphene/nanometer ferrite dispersion liquid; Added film-forming resin again and film coalescence aid disperses in sand mill, obtained aqueous electromagnetic shielding coating of the present invention.
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