CN103578678A - Magnetic iron-based graphite intercalation compound and preparation method thereof - Google Patents
Magnetic iron-based graphite intercalation compound and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a magnetic iron-based graphite intercalation compound and a preparation method thereof. The magnetic iron-based graphite intercalation compound is prepared from graphite micro powder through pre-oxidation, mixing of the graphite micro powder and ferric chloride, drying, intercalation, acid washing and reduction. According to the magnetic iron-based graphite intercalation compound and the preparation method thereof, used raw materials are easy to obtain, the method is simple and efficient, an obtained product has the good magnetic conductivity of iron-based magnetic materials and good electrical conductivity of graphite-based materials, excellent stability of the iron-based intercalation compound is achieved through the intercalation structure, and the magnetic iron-based graphite intercalation compound has good application prospect in the fields such as electromagnetic shielding, intelligent guided missile packaging materials, infrared absorption materials, and electrical conductive slurry due to all the characteristics of the magnetic iron-based graphite intercalation compound.
Description
Technical field
The present invention relates to a kind of Armco magnetic iron base graphite intercalation compound and preparation method thereof, this material is to take graphite microparticles as raw material, through pre-oxidation, iron chloride mix, dry, intercalation, pickling and reduction prepare, and belongs to electromagnetic material field.
Background technology
Electromagnetic shielding can reduce the electromagnetic radiation intensity of electronic apparatus, reduces electromagnetic radiation pollution, can also avoid electronic apparatus to be subject to extraneous electronic jamming simultaneously, avoids electronic apparatus to produce malfunction because of interference; Conventional electromagnetic shielding material has metallic plate, wire netting, loomage and shielding coating etc.According to the principle of electromagnetic shielding, the simple high-conductivity metal that adopts is as shielding material, and shielding is mainly the contribution of reflecting part, and the electromagnetic wave being reflected does not disappear, it can produce new radiation hazradial bundle to other region outside shielding area, forms secondary electromagnetic pollution.Absorbing material can electromagnetic wave absorption and is changed into heat energy, avoid this defect, common absorbing material, as ferrite, carbonyl iron dust etc., has higher magnetic loss tangent value, relies on magnetic hysteresis loss, raises magnetic polarization mechanism decay, the electromagnetic wave absorptions such as wall resonance, aftereffect loss; Other material, as material with carbon elements such as conductive black, graphite, has higher electrical loss tangent value, relies on electronic polarization or the interfacial polarization decay of medium, also can electromagnetic wave absorption, play electromagnetic shielding action.
Common electromagnetic shielding material mainly contains the materials such as metal Cu, Ag, Fe, Ni, and they have high conductivity and good mechanical property, and screening effectiveness is excellent, but density is large, perishable, be difficult for processing; Not enough in order to solve this class, people have studied various new electromagnetic shielding material, and what wherein attention rate was higher is polymer-based conduction or permeability magnetic material, from in form, an electromagnetic screen coating, its construction is easy, cost is low, but capability of electromagnetic shielding is relatively poor, stability is not enough.Another kind is structural type macromolecule, and it has, and easy to use, quality is light, the easy advantage such as machine-shaping, and application potential is huge, the raising but screening effectiveness and stability are still needed.
In the shielding material of polymer matrix, conventional conduction or magnetic conduction filler powder have silver powder, copper powder, graphite powder, metal nickel powder, carbonyl iron dust, ferrite powder etc.In these powders, silver powder screening effectiveness is excellent, stable performance, but cost higher (approximately 7000～10000 yuan/kilogram of prices); Copper powder initial performance is better, but easily oxidation, performance are unstable; Graphite powder stable performance, density is little, cost is low (10～50 yuan/kilogram), but conductivity is poor, screening effectiveness is general; Metal nickel powder stable performance, magnetic are better, moderate (200～800 yuan/kilogram), shielding properties be better, are the main flow fillers of current electromagnetic screen coating; Carbonyl iron dust magnetic is excellent, absorbing property is good, but cost is higher, oxidizable; Ferrite powder magnetic is better, absorbing property is better, but non-conductive, density is large, screening effectiveness is general.
Comprehensive sees, above-mentioned filler has the deficiency of self.From shielding principle, desirable electromagnetic shielding material should be the balance of conductivity and magnetic conductivity, namely requires the conductivity of shielding material and the magnetic conductivity all should be higher, and this material all has good capability of electromagnetic shielding in larger frequency range.Therefore the filler that, has high conductivity and a high magnetic permeability is the direction of electromagnetic shielding material development always.
Graphite is best a kind of of electric conductivity in material with carbon element, and its linear conductivity is about 10
5～10
4s/cm.The graphite of take can prepare graphite layers intercalation compound (graphite intercalation compounds, be called for short GIC) as raw material, and its Conductivity Ratio raw material graphite is high one more than the order of magnitude, and part GIC is (as SbF
5-GIC) conductivity is higher than metallic copper, and they are good electromagnetic shielding materials, but stability, weatherability are very poor, there is no using value.The compound between graphite layers FeCl of iron chloride intercalation
3-GIC has higher structural stability in air, possesses good actual application value, generally by methods such as two chamber methods and molten salt growth methods, prepares; The method utilization of two chambers is placed on respectively the FeCl at sealing glass reactor two ends
3(steam) reacts with graphite, and the rank index of GIC is controlled, but device is complicated, the reaction time is long, temperature is high.Molten salt growth method (also claiming liquid phase method) is the preparation method of tool using value, and it is the molten salt system that utilizes two or more material to form, and realizes intercalation at lower temperature, installs simple efficiency high, is applicable to extensive preparation.Document [charcoal element technology, 1990,5,7] has been introduced a kind of molten salt growth method and has been prepared FeCl
3the method of-GIC, this method is directly by graphite and anhydrous FeCl
3mix, be heated to FeCl
3more than fusing point, the liquid phase FeCl of fusing
3directly react and obtain FeCl with graphite
3-GIC, but need high vacuum, anhydrous and oxygen-free environment.Document [chemistry and bioengineering, 2006,5,9] has reported that a kind of fused salt mixt legal system is for CoCl
2-FeCl
3the method of-GIC, is also to pack glass container into, vacuumizes rear inflated with nitrogen, sealing by fusing sealing after assurance anaerobic anhydrous state, and reaction temperature is high, the reaction time is long (8h).Document [novel charcoal material, 2000,1,18] has also been reported similar approach.Comprehensive literature, molten salt growth method is prepared FeCl
3-GIC needs sealing by fusing in glass reactor, under anhydrous and oxygen free condition, reacts and obtains, and these operate in complicated operation in actual application, difficulty is large.
FeCl
3-GIC has higher conductivity, but there is no magnetic, from the angle of electromagnetic shielding, sees not satisfactory.From principle, magnetic nano-substance also can be implanted in the space of graphite layers, this can improve the conductivity of graphite on the one hand, also can utilize the isolated magnetic nano-substance of graphite linings and external environment, avoid because the problems such as oxidation lose magnetism, the graphite of the magnetisable material intercalation of preparation had both had good conductivity like this, had again good magnetic and stability, will be a kind of good electromagnetic shielding material, in field of compound material such as electromagnetic screen coatings, will have good application potential.
The present invention be take graphite microparticles as raw material, through pre-oxidation, iron chloride mix, dry, intercalation, pickling and reduction process prepare Armco magnetic iron base graphite intercalation compound.Raw material is cheaply easy to get, method is simply efficient, products obtained therefrom has magnetic conductivity and the good conductivity of graphite substrate that ferrous metals is good, its intercalation configuration is given again the stability of magnetic intercalation compound excellence, also have that graphite substrate particle diameter is adjustable simultaneously, light weight, be easy to the characteristics such as dispersion, make this Armco magnetic iron base graphite intercalation compound have good application prospect in fields such as electromagnetic shielding, intelligent missile packaging material, infrared absorbing material, electrocondution slurries.
Summary of the invention
The object of the invention is to disclose a kind of Armco magnetic iron base graphite intercalation compound and technical scheme simply efficient, that can prepare on a large scale thereof.
Technical scheme of the present invention is:
Take graphite microparticles and iron chloride as raw material, through pre-oxidation, mixing, dry, heating intercalation, pickling, obtain iron-based graphite intercalation compound, then obtain Armco magnetic iron base graphite intercalation compound through reduction.
Iron-based intercalation compound before above-mentioned reduction is non-stoichiometric FeOCl, the atomic ratio of three kinds of elements is: Fe:O:Cl=1:(0.05～0.7): (0.05～0.6), this intercalation compound is thermally-stabilised good, can under the condition that has water aerobic, operate, avoid the steps such as conventional molten salt growth method vacuum and glass head seal thereof, simplified preparation process and the device of graphite intercalation compound.
Above-mentioned iron-based graphite intercalation compound is reduced in reducing atmosphere, after cooling Armco magnetic iron base graphite intercalation compound, this reduction process does not need to reduce completely, as long as give iron-based graphite intercalation compound certain magnetic, technique is simply efficient.
Because above-mentioned magnetic iron-based intercalation compound is present in graphite layers, completely cut off external environment condition, avoided the adverse effect because of external environment effect magnetic decline variation, give the material stability of excellence in actual use.
A kind of Armco magnetic iron base graphite intercalation compound the present invention relates to and preparation method thereof, its preparation process comprises following concrete steps:
(1) pre-oxidation: graphite microparticles is fully mixed with the strong oxidant solution of 0.5～10 times of quality, and filtration drying after standing 1～24 hour, obtains the graphite microparticles of pre-oxidation;
(2) iron chloride is mixed and dry: after the graphite microparticles of pre-oxidation is added to suitable quantity of water, mix with the iron chloride of metering ratio, 80～150 ℃ are dried 1～24 hour, obtain the mixture of iron chloride and graphite microparticles;
(3) intercalation and pickling: the mixture of above-mentioned iron chloride and graphite microparticles is placed in to tubular heater, in inert atmosphere, 300～500 ℃ of heat treatment is 0.5～10 hour, after cooling taking-up, with watery hydrochloric acid and deionized water, wash 2～3 times successively, after being dried, obtain iron-based graphite intercalation compound;
(4) reduction: gained iron-based graphite intercalation compound is placed in to tubular heater, in reducing atmosphere 320～600 ℃ reduction 0.5～10 hour, cooling after both Armco magnetic iron base graphite intercalation compound product.
Graphite microparticles described in step (1) can be that various particle diameters are micron-sized various graphite composite powder, needn't limit its concrete particle size, as long as be convenient to follow-up practical application and inexpensive.
Strong oxidizer described in step (1) is one or several the mixture in red fuming nitric acid (RFNA), perchloric acid, clorox, hydrogen peroxide, potassium permanganate, the object of use strong oxidizer is herein the marginal portion of graphite oxide interlayer, reduce the difficulty of follow-up intercalation process, so the ratio of graphite powder and strong oxidizer needn't strictly limit, as long as can be by graphite powder submergence, guarantee that the two fully contacts, consider convenience and the economy of practical operation, the mass ratio of graphite microparticles and strong oxidant solution is 0.5～10 proper.The time of pre-oxidation determines according to the oxidability of strong oxidizer, and the time that oxidizability is strong is short, and weak time of oxidizability can proper extension, consider, oxidization time be 1～24 hour proper.
The metering of the graphite in step (2) after iron chloride and oxidation is than the exponent number that has determined graphite intercalation compound, content and the magnetic thereof of iron in final Armco magnetic iron base graphite intercalation compound have namely been determined, therefore can change according to actual needs, iron content is high in Armco magnetic iron base graphite intercalation compound, magnetic good for iron chloride ratio height, and vice versa; Consider magnetic and economy, the mass ratio of iron chloride and graphite is 1:(0.1～20) time proper.
The factors such as baking temperature and time described in step (2) determine according to iron chloride consumption, and greatly baking temperature is high, drying time is long for iron chloride consumption, and vice versa, comprehensive preparation efficiency, 80～150 ℃ dry 1～24 hour proper.
Inert atmosphere described in step (3) is not have too much oxygen element when making intercalation to enter intercalation compound, so its kind needn't strictly limit, N
2, Ar, He, CO
2in one or several mixture all can, from economic angle, consider N
2best.
300～500 ℃ of heat treatment 0.5～10 hour in inert atmosphere of material described in step (3), this process intercalation compound enters graphite layers, must be heated to uniform temperature and keep a period of time, the low intercalation of heating-up temperature speed is slow, for guaranteeing that the abundant required time of intercalation just should extend, vice versa.Intercalation temperature can not be lower than 300 ℃, otherwise cannot obtain intercalation compound, can not be higher than 500 ℃, otherwise intercalation compound is de-, insert seriously, consider, 300～500 ℃ of heat treatment 0.5～10 hour is proper, and the iron-based intercalation compound intercalation now obtaining is more abundant, and subsequent product magnetic is better.
Material described in step (3) washs 2～3 times at cooling rear watery hydrochloric acid and the deionized water used, object is to dissolve to remove not intercalation and enter the compound of graphite layers, so unlike limiting sour kind and concentration, but for fear of bringing other ion into, hydrochloric acid is better.Guaranteeing under the sufficient prerequisite of washing washing times 2-3 time.
In step (4), gained iron-based graphite intercalation compound is placed in to tubular heater, in reducing atmosphere, 320～600 ℃ are reduced 0.5～10 hour, this step object is iron-based graphite intercalation compound to reduce, give its magnetic, by its all or part of Armco magnetic iron based compound that is reduced into, conventional reducibility gas can, consider that economy reducing gas is H
2, CO, NH
3in one or several mixture.Reduction temperature is proper between 320～600 ℃, too low cannot reduction, and too high easily de-inserting, 0.5～10 hour recovery time is proper, so not only economy but also efficient.
The Armco magnetic iron base graphite intercalation compound pattern preparing and performance characterize by classical method, for example, with the pattern of sem observation Armco magnetic iron base graphite intercalation compound, result shows that gained Armco magnetic iron base graphite intercalation compound is all in graphite layers.By the magnetic of vibrating specimen magnetometer test material, result shows that its specific saturation magnetization is 20～150emu/g, and coercive force is 30～160Oe, and magnetic is good.The gained Armco magnetic iron base graphite intercalation compound of take is filler, it is mixed to dispersion with coating matrix, applies into the annular membrane (thick 10 microns) of specific thickness, at its electromagnet shield effect of 0.3MHz～2GHz scope build-in test, is 30～50dB, excellent performance.
In sum, technique effect of the present invention is obvious.It is raw material that graphite microparticles and iron chloride are take in the present invention, by molten salt growth method, through pre-oxidation, mixing, dry, heating intercalation, pickling, obtains iron-based graphite intercalation compound, then obtains Armco magnetic iron base graphite intercalation compound through reduction.Method is simply efficient, raw material is inexpensive, gained magnetic iron-based intercalation compound is present in graphite layers, completely cut off external environment, avoid losing magnetism because of oxidation, stability and weatherability are good, and this material has the magnetic of the good conductivity of graphite and Fe-base compound concurrently simultaneously, are expected to be widely used in the fields such as electromagnetic shielding, intelligent missile packaging material, infrared absorbing material, electrocondution slurry.
Accompanying drawing explanation
The typical iron-based graphite intercalation compound of Fig. 1 scanning electron microscopy (SEM) photo
Iron-based graphite intercalation compound scanning electron microscopy (SEM) photo of the typical mist reduction of Fig. 2
The typical iron-based graphite intercalation compound of Fig. 3 X-ray diffraction (XRD) collection of illustrative plates
The typical iron-based graphite intercalation compound of Fig. 4 magnetic property (vibration magnetic strength instrumentation is determined magnetic hysteresis loop)
Embodiment
For the present invention is described better, attached embodiment is as follows.It is emphasized that embodiment and do not mean that scope of the present invention is limited in the condition of embodiment narration, the object of embodiment is further to set forth content of the present invention and feasibility thereof.
Embodiment 1:
By the nitric acid dousing of 6mol/L 12 hours for the aquadag of 10g4～6 μ m, deionized water washing for filtering, dry after and 10g FeCl
3.6H
2o mixes (quality is than iron/graphite=1/1), adds suitable quantity of water and stirs evenly and obtain pasty mixture, and 80 ℃ dry ground after 10 hours, in blanket of nitrogen, be heated to 300 ℃, be incubated 10 hours, cooling taking-up is filtered with 5% hydrochloric acid solution water-bath washing afterwards, deionized water washing, dry after at H
2atmosphere is heated to 320 ℃ in enclosing, be incubated 10 hours, and cooling taking-up had both obtained product, and wherein metal Ferrum content is 17%.
Products obtained therefrom is added in acrylic resin soln and is uniformly dispersed, with silk screen printing circlewise, at its electromagnet shield effect of 1MHz～2GHz scope build-in test, reach 30～50dB.
Embodiment 2:
Use the clorox of 1mol/L to soak 18 hours the aquadag of 10g4～6 μ m, deionized water washing for filtering, dry rear and 1g FeCl
3.6H
2o mixes (quality is than iron/graphite=1/10), adds suitable quantity of water and stirs evenly and obtain pasty mixture, and 100 ℃ dry ground after 9 hours, in argon atmospher, be heated to 300 ℃, be incubated 2 hours, be warming up to 400 ℃, be incubated 3 hours, cooling taking-up is filtered with 5% hydrochloric acid solution water-bath washing afterwards, deionized water washing is heated to 600 ℃ after being dried in CO atmosphere is enclosed, and is incubated 0.5 hour, cooling taking-up had both obtained product, and wherein metal Ferrum content is 2%.
Products obtained therefrom is added in acrylic resin soln and is uniformly dispersed, with silk screen printing circlewise, at its electromagnet shield effect of 1MHz～2GHz scope build-in test, reach 32～48dB.
Embodiment 3:
Use the perchloric acid of 1mol/L to soak 1 hour the aquadag of 10g4～6 μ m, deionized water washing for filtering, dry rear and 20g FeCl
3.6H
2o mixes (quality is than iron/graphite=1/0.5), adding suitable quantity of water stirs evenly and obtains pasty mixture, 110 ℃ of dry grindings after 7 hours, in helium-atmosphere, be heated to 300 ℃, be incubated 1 hour, be warming up to 450 ℃, be incubated 2 hours, cooling taking-up is filtered with 5% hydrochloric acid solution water-bath washing afterwards, deionized water washing, dry after at NH
3atmosphere is heated to 350 ℃ in enclosing, be incubated 8 hours, and cooling taking-up had both obtained product, and wherein metal Ferrum content is 29%.
Products obtained therefrom is added in acrylic resin soln and is uniformly dispersed, with silk screen printing circlewise, at its electromagnet shield effect of 1MHz～2GHz scope build-in test, reach 30～46dB.
Embodiment 4:
Use the clorox of 2mol/L to soak 8 hours the aquadag of 10g4～6 μ m, deionized water washing for filtering, dry rear and 3.3g FeCl
3.6H
2o mixes (quality is than iron/graphite=1/3), adds suitable quantity of water and stirs evenly and obtain pasty mixture, and 120 ℃ dry ground after 6 hours, in carbon dioxide atmosphere, be heated to 350 ℃, be incubated 7 hours, cooling taking-up is filtered with 5% hydrochloric acid solution water-bath washing afterwards, deionized water washing, dry after at H
2/ NH
3(1/1) in gaseous mixture atmosphere, be heated to 300 ℃, be incubated 1 hour, be warming up to 450 ℃, be incubated 5 hours, cooling taking-up had both obtained product, and wherein metal Ferrum content is 6%.
Products obtained therefrom is added in acrylic resin soln and is uniformly dispersed, with silk screen printing circlewise, at its electromagnet shield effect of 1MHz～2GHz scope build-in test, reach 30～50dB.
Embodiment 5:
By 15% hydrogen peroxide dipping 24 hours for the aquadag of 10g4～6 μ m, deionized water washing for filtering, dry after and 2.5g FeCl
3.6H
2o mixes (metering is than iron/graphite=1/4), adds suitable quantity of water and stirs evenly and obtain pasty mixture, and 125 ℃ dry ground after 5 hours, in blanket of nitrogen, be heated to 480 ℃, be incubated 1 hour, cooling taking-up is filtered with 5% hydrochloric acid solution water-bath washing afterwards, deionized water washing, dry after at H
2in/CO (1/1) gaseous mixture atmosphere, be heated to 300 ℃, be incubated 1 hour, be warming up to 550 ℃, be incubated 3 hours, cooling taking-up had both obtained product, and wherein metal Ferrum content is 4.9%.
Products obtained therefrom is added in acrylic resin soln and is uniformly dispersed, with silk screen printing circlewise, at its electromagnet shield effect of 1MHz～2GHz scope build-in test, reach 35～50dB.
Embodiment 6:
Use the potassium permanganate of 1mol/L to soak 3 hours the aquadag of 10g4～6 μ m, deionized water washing for filtering, dry rear and 2g FeCl
3.6H
2o mixes (metering is than iron/graphite=1/5), adds suitable quantity of water and stirs evenly and obtain pasty mixture, and 130 ℃ dry ground after 4 hours, in argon atmospher, be heated to 320 ℃, be incubated 8 hours, cooling taking-up is filtered with 5% hydrochloric acid solution water-bath washing afterwards, deionized water washing, dry after at CO/NH
3(1/1) in gaseous mixture atmosphere, be heated to 300 ℃, be incubated 1 hour, be warming up to 400 ℃, be incubated 6 hours, cooling taking-up had both obtained product, and wherein metal Ferrum content is 3.9%.
Products obtained therefrom is added in acrylic resin soln and is uniformly dispersed, with silk screen printing circlewise, at its electromagnet shield effect of 1MHz～2GHz scope build-in test, reach 30～48dB.
Embodiment 7:
Use the perchloric acid of 2mol/L to soak 18 hours the aquadag of 10g4～6 μ m, deionized water washing for filtering, dry rear and 100g FeCl
3.6H
2o mixes (metering is than iron/graphite=1/0.1), adds suitable quantity of water and stirs evenly and obtain pasty mixture, and 140 ℃ dry ground after 2 hours, in carbon dioxide atmosphere, be heated to 380 ℃, be incubated 6 hours, cooling taking-up is filtered with 5% hydrochloric acid solution water-bath washing afterwards, deionized water washing, dry after at H
2in/CO (1/1) gaseous mixture atmosphere, be heated to 300 ℃, be incubated 1 hour, be warming up to 500 ℃, be incubated 4 hours, cooling taking-up had both obtained product, and wherein metal Ferrum content is 67%.
Products obtained therefrom is added in acrylic resin soln and is uniformly dispersed, with silk screen printing circlewise, at its electromagnet shield effect of 1MHz～2GHz scope build-in test, reach 32～45dB.
Embodiment 8:
By the nitric acid dousing of 6mol/L 12 hours for the aquadag of 10g4～6 μ m, deionized water washing for filtering, dry after and 0.5g FeCl
3.6H
2o mixes (metering is than iron/graphite=1/20), adds suitable quantity of water and stirs evenly and obtain pasty mixture, and 150 ℃ dry ground after 0.5 hour, in blanket of nitrogen, be heated to 500 ℃, be incubated 0.5 hour, cooling taking-up is filtered with 5% hydrochloric acid solution water-bath washing afterwards, deionized water washing, dry after at H
2/ NH
3(1/1) in gaseous mixture atmosphere, be heated to 300 ℃, be incubated 1 hour, be warming up to 450 ℃, be incubated 5 hours, cooling taking-up had both obtained product, and wherein metal Ferrum content is 1%.
Products obtained therefrom is added in acrylic resin soln and is uniformly dispersed, with silk screen printing circlewise, at its electromagnet shield effect of 1MHz～2GHz scope build-in test, reach 35～50dB.
Claims (7)
1. Armco magnetic iron base graphite intercalation compound and preparation method thereof, it is characterized in that this Armco magnetic iron base graphite intercalation compound is to take graphite microparticles as raw material, through pre-oxidation, iron chloride mix, dry, intercalation, pickling and reduction process prepare, wherein the iron-based intercalation compound before reduction is non-stoichiometric FeOCl, and the atomic ratio of three kinds of elements is: Fe:O:Cl=1:(0.05～0.7): (0.05～0.6).
2. according to a kind of Armco magnetic iron base graphite intercalation compound of claim 1 and preparation method thereof, it is characterized in that being prepared by following detailed process:
(1) pre-oxidation: graphite microparticles is fully mixed with the strong oxidant solution of 0.5～10 times of quality, and filtration drying after standing 1～24 hour, obtains the graphite microparticles of pre-oxidation;
(2) iron chloride mixes with dry: after the graphite microparticles of pre-oxidation is added to suitable quantity of water, mix with the iron chloride of metering ratio, 80～150 ℃ are dried 1～24 hour, obtain the mixture of iron chloride and graphite microparticles;
(3) intercalation and pickling: the mixture of above-mentioned iron chloride and graphite microparticles is placed in to tubular heater, in inert atmosphere, 300～500 ℃ of heat treatment is 0.5～10 hour, after cooling taking-up, with watery hydrochloric acid and deionized water, wash 2～3 times successively, after being dried, obtain iron-based graphite intercalation compound;
(4) reduction: gained iron-based graphite intercalation compound is placed in to tubular heater, and 320～600 ℃ of reduction are 0.5～10 hour in reducing atmosphere, after cooling Armco magnetic iron base graphite intercalation compound.
3. according to a kind of Armco magnetic iron base graphite intercalation compound described in claim 1～2 and preparation method thereof, it is characterized in that described strong oxidizer is one or several the mixture in red fuming nitric acid (RFNA), perchloric acid, clorox, hydrogen peroxide, potassium permanganate.
4. according to a kind of Armco magnetic iron base graphite intercalation compound described in claim 1～2 and preparation method thereof, it is characterized in that described iron chloride and the mass ratio of graphite are 1:(0.1～20).
5. according to a kind of Armco magnetic iron base graphite intercalation compound described in claim 1～2 and preparation method thereof, it is characterized in that described inert atmosphere is N
2, Ar, He, CO
2in one or several mixture.
6. according to a kind of Armco magnetic iron base graphite intercalation compound described in claim 1～2 and preparation method thereof method, it is characterized in that described reducing atmosphere is H
2, CO, NH
3in one or several mixture.
7. according to a kind of Armco magnetic iron base graphite intercalation compound described in claim 1 or 2～6 and preparation method thereof, it is characterized in that described iron-based graphite intercalation compound can be used for electromagnetic shielding, intelligent missile packaging material, infrared absorbing material, electrocondution slurry.
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| CN103881139B (en) * | 2014-03-10 | 2016-10-19 | 高碑店市顺新化工有限公司 | A kind of multi-functional compound between graphite layers and preparation method and application |
| CN107934945A (en) * | 2017-12-07 | 2018-04-20 | 西南交通大学 | A kind of method for preparing magnetic graphene using molysite gas phase intercalation and microwave technology |
| CN107934945B (en) * | 2017-12-07 | 2020-12-18 | 西南交通大学 | Method for preparing magnetic graphene by utilizing ferric salt gas phase intercalation and microwave technology |
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