CN107265449A - A kind of preparation method for being electromagnetically shielded graphene - Google Patents
A kind of preparation method for being electromagnetically shielded graphene Download PDFInfo
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- CN107265449A CN107265449A CN201710454790.4A CN201710454790A CN107265449A CN 107265449 A CN107265449 A CN 107265449A CN 201710454790 A CN201710454790 A CN 201710454790A CN 107265449 A CN107265449 A CN 107265449A
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Abstract
The present invention provides a kind of preparation method for being electromagnetically shielded graphene, and step is（1）Clean graphenic surface；（2）Carry out high temperature oxidation process；（3）Graphene is impregnated in nickel nitrate solution, dries, operates repeatedly, to nickel：The mass ratio of graphene is 13 19:85 92, lead to hydrogen reduction, produce.Graphene is impregnated nickel nitrate by the present invention, restores, porous nickel dam is formd in graphenic surface, strengthen with the bond strength of other materials, improve the shielding properties of graphene, decay resistance is also improved, the method is simple, and obtained graphene shield effectiveness is good, good corrosion resistance.
Description
Technical field
The present invention relates to technical field of graphene, more particularly to a kind of preparation method for being electromagnetically shielded graphene.
Background technology
Ocean is richly stored with natural resources, reasonable development and using ocean firstly the need of in face of marine corrosion problem.
Marine facility and ship are chronically at the oxygen-enriched salt fog of alternation of wetting and drying, the environment of high ultraviolet, and etching problem is extremely serious.Cause
This, reasonable utilization marine anticorrosion erosion technology, the generation for reducing disaster accident improves the safety of ship and ocean platform facility
Property, extending its service life has profound meaning.Graphene and graphite nano plate are emerging two-dimensional nano-carbon materials, are had
The structure of lamellar, has good stability and barrier to water, oxygen and ion, during filler as traditional coating, can be with
Good physical shielding effect is played, so as to improve the decay resistance of organic coating.Herein respectively with thermal reduction graphene and
Graphite nano plate makees filler, using epoxy resin as matrix, have studied the design feature of thermal reduction graphene and graphite nano plate, with
And their decay resistances and mechanism in coating.Using graphite nano plate as filler, graphite nano plate is have studied in coating
In decay resistance and mechanism.The graphite nano plate surface unusual light of preparation, the thickness of lamella is about 50nm, lamella it is straight
Footpath is about 2-10 μm.The graphite nano plate anticorrosive paint of different content, electrification are directly prepared for using graphite nano plate as filler
Learn and resistance to neutral salt spray test shows, preferably, corrosion potential is -435m V to 10% graphite nano plate corrosion resistance coating of addition, from
Corrosion electric current density is 0.055 μ A/cm2.Graphite nano plate is modified by coupling agent, and is prepared for modified graphite nanometer
Piece coating, the corrosion resistance for adding 10% modified graphite nanometer sheet coating is best, and corrosion potential is -416m V, and corrosion current is close
Spend for 0.032 μ A/cm2.Graphite nano plate forms physical barriers in coating, hinders the infiltration of corrosive medium.With thermal reduction stone
Black alkene is filler, have studied decay resistance and mechanism of the graphite nano plate in coating.XRD, Raman, XPS and SEM decile
Analysis shows, some oxy radicals is remained on thermal reduction graphene, the thickness of lamella is about 40nm, and lamella diameter is about 2-5 μm.Directly
Connect the graphene coating that different content is prepared for using thermal reduction graphene as filler, electrochemistry and the table of resistance to neutral salt spray test
Bright, preferably, corrosion potential is -428m V to 1.5% thermal reduction graphene corrosion resistance coating of addition, and corrosion current density is
0.058μA/cm2.Thermal reduction graphene is modified by coupling agent, and is prepared for modified graphene coating, addition 2% changes
Property graphite ene coatings corrosion resistance preferably, corrosion potential be -360m V, corrosion current density be 0.034 μ A/cm2.Heat is also
Former graphene is uniformly dispersed in the base, hinder corrosive medium infiltration, it is coupling agent modified after improve its in coating point
Property and the interface binding power with resin are dissipated, corrosion potential improves 68m V, and corrosion current density reduces 58.6%.This
Text further study influence of the reduction temperature to graphene corrosion resistance of coating energy.Respectively in 450 DEG C, 750 DEG C, 1050 DEG C of temperature
Under degree, different reduction temperature graphenes are prepared for, XPS tests show that its C/O is respectively 6.2,7.4,8.4;Can be with from SEM photograph
Find out, with the rise of reduction temperature, the extent of exfoliation of graphene is higher, and form is progressively changed into sheet from hollow spheres.Electricity
Test chemical shows that the graphene anticorrosion with coat performance of 1050 DEG C of reduction is best, although can retain under relatively low reduction temperature
More oxy radicals, but the structure of lamellar could not be peeled off into, therefore the effect reduction of its physical barriers, antiseptic property drop
It is low.
《Graphene（Graphite nano plate）The research of/epoxy resin ship coating antiseptic property》One text directly adds graphene
Enter in coating, the binding ability with coating is poor, easily produces gap, causes coating to ftracture, corrode, the method for nickel plating is excessively multiple
It is miscellaneous, it is necessary to improve.
The content of the invention
The object of the invention is exactly that there is provided a kind of preparation side for being electromagnetically shielded graphene in order to make up the defect of prior art
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method for being electromagnetically shielded graphene, step is
（1）Clean graphenic surface；
（2）Carry out high temperature oxidation process；
（3）Graphene is impregnated in nickel nitrate solution, dries, operates repeatedly, to nickel：The mass ratio of graphene is 13-19:
85-92, leads to hydrogen reduction, produces.
It is described cleaning graphene method be：
（1）Graphene is put into water, placed into supersonic wave cleaning machine, detergent is added and cleans 10-20 minutes, cleaned with water
The detergent of residual；
（2）Cleaned 5-10 minutes in 60-70 DEG C of aqueous slkali, residual alkali lye is cleaned with water.
The method of the high temperature oxidation process is：Cleaned graphene is inserted in Muffle furnace, 930-960 is warming up to
DEG C, 5-6 hours are incubated, furnace cooling.
Graphene dipping process in nickel nitrate solution is：Graphene is impregnated in nickel nitrate solution, 2- is stood
5min, is at the uniform velocity pulled out, and is dried at 140-150 DEG C, is calcined 1-2 hours at 500-550 DEG C, and heating rate is 5-6 DEG C/min,
Furnace cooling.
The concentration of the nickel nitrate solution, 20-25g/L, solvent is water, liquefied ammonia, one kind of multiple mixtures of ethanol.
Graphene is dried at 120-140 DEG C, then logical hydrogen reduction.
It is an advantage of the invention that：Graphene is impregnated nickel nitrate by the present invention, is restored, is formd in graphenic surface porous
Nickel dam, strengthen with the bond strength of other materials, improve the shielding properties of graphene, decay resistance is also improved,
The method is simple, and obtained graphene effectiveness is good, good corrosion resistance, electric conductivity enhancing.
Embodiment
A kind of preparation method for being electromagnetically shielded graphene, step is
（1）Clean graphenic surface；
（2）Carry out high temperature oxidation process；
（3）Graphene is impregnated in nickel nitrate solution, dries, operates repeatedly, to nickel：The mass ratio of graphene is 16:90, lead to
Hydrogen reduction, is produced.
It is described cleaning graphene method be：
（1）Graphene is put into water, placed into supersonic wave cleaning machine, detergent is added and cleans 15 minutes, clean residual with water
The detergent stayed；
（2）Cleaned 8 minutes in 65 DEG C of aqueous slkali, residual alkali lye is cleaned with water.
The method of the high temperature oxidation process is：Cleaned graphene is inserted in Muffle furnace, 940 DEG C, guarantor are warming up to
Temperature 5 hours, furnace cooling.
Graphene dipping process in nickel nitrate solution is：Graphene is impregnated in nickel nitrate solution, stood
3min, is at the uniform velocity pulled out, and is dried at 140 DEG C, is calcined 1 hour at 500 DEG C, and heating rate is 5 DEG C/min, furnace cooling.
The concentration of the nickel nitrate solution, 23g/L, solvent is water, liquefied ammonia, one kind of multiple mixtures of ethanol.
Graphene is dried at 130 DEG C, then logical hydrogen reduction.
Claims (6)
1. a kind of preparation method for being electromagnetically shielded graphene, it is characterised in that：Step is
（1）Clean graphenic surface；
（2）Carry out high temperature oxidation process；
（3）Graphene is impregnated in nickel nitrate solution, dries, operates repeatedly, to nickel：The mass ratio of graphene is 13-19:
85-92, leads to hydrogen reduction, produces.
2. the preparation method of the electromagnetic shielding graphene according to claim 1, it is characterised in that：The cleaning graphene
Method be：
（1）Graphene is put into water, placed into supersonic wave cleaning machine, detergent is added and cleans 10-20 minutes, cleaned with water
The detergent of residual；
（2）Cleaned 5-10 minutes in 60-70 DEG C of aqueous slkali, residual alkali lye is cleaned with water.
3. the preparation method of the electromagnetic shielding graphene according to claim 1, it is characterised in that：At the high-temperature oxydation
The method of reason is：Cleaned graphene is inserted in Muffle furnace, 930-960 DEG C is warming up to, 5-6 hours are incubated, furnace cooling.
4. the preparation method of electromagnetic shielding graphene according to claim 1, it is characterised in that：The graphene is in nitric acid
Dipping process is in nickel solution：Graphene is impregnated in nickel nitrate solution, 2-5min is stood, at the uniform velocity pulls out, at 140-150 DEG C
Lower drying, is calcined 1-2 hours at 500-550 DEG C, and heating rate is 5-6 DEG C/min, furnace cooling.
5. the preparation method of the electromagnetic shielding graphene according to claim 1, it is characterised in that：The nickel nitrate solution
Concentration, 20-25g/L, solvent be water, liquefied ammonia, one kind of multiple mixtures of ethanol.
6. the preparation method of the electromagnetic shielding graphene according to claim 1, it is characterised in that：By graphene in 120-
Dried at 140 DEG C, then logical hydrogen reduction.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710454790.4A CN107265449A (en) | 2017-06-16 | 2017-06-16 | A kind of preparation method for being electromagnetically shielded graphene |
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| CN201710454790.4A CN107265449A (en) | 2017-06-16 | 2017-06-16 | A kind of preparation method for being electromagnetically shielded graphene |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102218540A (en) * | 2010-04-14 | 2011-10-19 | 韩国科学技术院 | Graphene/metal nanocomposite powder and method for manufacturing same |
| CN103787328A (en) * | 2014-03-11 | 2014-05-14 | 华南师范大学 | Modified grapheme preparation method |
| CN104028269A (en) * | 2014-06-20 | 2014-09-10 | 南京工业大学 | Graphene-loaded metal nanocomposite, preparation method and application |
-
2017
- 2017-06-16 CN CN201710454790.4A patent/CN107265449A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102218540A (en) * | 2010-04-14 | 2011-10-19 | 韩国科学技术院 | Graphene/metal nanocomposite powder and method for manufacturing same |
| CN103787328A (en) * | 2014-03-11 | 2014-05-14 | 华南师范大学 | Modified grapheme preparation method |
| CN104028269A (en) * | 2014-06-20 | 2014-09-10 | 南京工业大学 | Graphene-loaded metal nanocomposite, preparation method and application |
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Application publication date: 20171020 |
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