CN105000886A - Macroscopic three-dimensional ultralight Fe3O4 doped graphene aerogel composite material and preparation method - Google Patents

Macroscopic three-dimensional ultralight Fe3O4 doped graphene aerogel composite material and preparation method Download PDF

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CN105000886A
CN105000886A CN201510405177.4A CN201510405177A CN105000886A CN 105000886 A CN105000886 A CN 105000886A CN 201510405177 A CN201510405177 A CN 201510405177A CN 105000886 A CN105000886 A CN 105000886A
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graphene
graphene aerogel
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graphene oxide
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CN105000886B (en
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郑修成
孟婧珂
刘玉山
索阳
关新新
张建民
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Zhengzhou University
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Abstract

The invention belongs to the technical field of functional materials and relates to a macroscopic three-dimensional ultralight Fe3O4 doped graphene aerogel composite material and a preparation method. According to the preparation method, firstly, expanded graphite powder is taken as a raw material, graphene oxide is prepared with an improved Hummers method, and ferric trichloride is thermally hydrolyzed to prepare ferric hydroxide colloid; secondly, the ferric hydroxide colloid is dropwise added into a graphene oxide solution, and a hydrothermal reduction reaction is performed to obtain Fe3O4 doped graphene aerogel; and finally, hydrothermal treatment by ammonia water and vacuum freeze-drying are performed to obtain the macroscopic three-dimensional ultralight Fe3O4 doped graphene aerogel composite material. In percentage by weight, the Fe3O4 content is 0-65% and the balance is graphene aerogel. The synthetic method for the Fe3O4 doped graphene aerogel composite material is simple, feasible, easy to control, small in specific gravity, large in surface area and outstanding in porous characteristic, and can be used in the fields of sewage treatment, stealth, biological medicines, new energy, electronic materials and the like.

Description

A kind of macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite and preparation method
Technical field
The invention belongs to technical field of function materials, particularly a kind of macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite and preparation method.
Background technology
As the ferrite comparatively early found by the mankind and use, Fe 3o 4there is the character such as unique magnetics and electricity, and preparation method is relatively simple, chemical stability is good, is widely used as magneticsubstance, catalyzer, abrasive material, sewage-treating agent, special electrode etc.Graphene is a kind of novel carbon material after soccerballene, carbon nanotube, is sp 2the carbon atom of hydridization arrange in hexagonal lattice form sheet individual layer, have excellent electricity, machinery and chemical property.But the mode of two-dimensional graphene easily by parallel is stacking, this just substantially reduces its specific surface area, conventional Fe 3o 4also it is not enough to there is the little grade of specific surface area in class.The reunion between Graphene effectively can be solved based on graphene aerogel (graphene aerogel, GA) that is three-dimensional netted and vesicular structure feature.Compared with Graphene, the large size material that GA is a kind of bigger serface, external morphology is adjustable, shows more excellent physicochemical property.On the one hand, sensor and catalytic applications can provide number of ways for ion and molecular diffusion and electronics transport; On the other hand, its vesicular structure is the ideal stent of organic or inorganic nano material.Thus GA sill has a wide range of applications.
At present, more existing reports about GA based composites, as GA load SnO 2(CN 104143631 A), N doping GA load C oO x(CN 104319395 A), GA supported V 2o 5(CN 104437277 A).But have no relevant macroscopic three dimensional Fe 3o 4the report of doped graphene aerogel ultra light composite and preparation method, and by Fe 3o 4be complex as with GA and have concurrently and the functional materials of characteristic both improving, in sewage disposal, stealthy, biological medicine, new forms of energy and electronic material etc., have potential application.
Summary of the invention
The object of this invention is to provide a kind of macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite and preparation method, described matrix material has concurrently and improves Fe 3o 4with the respective characteristic of graphene aerogel, solve current block Ferrite Material specific surface area little and graphene-based material and the problem such as easily to reunite.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite, Fe by weight percentage 3o 4content be 0-65%, and be not 0%, Fe 3o 4content be preferably 25-55%, surplus is graphene aerogel.
Further, described a kind of macroscopic three dimensional Fe 3o 4the density of@graphene aerogel ultra light composite is 0.05-0.10g/cm 3, mean pore size is 3.00-7.00nm, total pore volume is 0.12-0.52cm 3/ g, specific surface area are 180-400m 2/ g.
Further, described a kind of macroscopic three dimensional Fe 3o 4the macroscopic three dimensional structure of@graphene aerogel ultra light composite is columnar structure, diameter 1-3cm, height 2-7cm.
A kind of macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite, its preparation method comprises the following steps:
Step one, pretreating graphite powder:
First by concentrated nitric acid and the vitriol oil by volume 1: (1-5), be preferably 1: 3 and be mixed and made into mix acid liquor, at room temperature Graphite Powder 99 is put into mix acid liquor, (5-12) part Graphite Powder 99 is put into according to 100 parts of mix acid liquors, stir 16-32h, be preferably 100 parts of mix acid liquors and put into 10 parts of Graphite Powder 99s, stir 24h, then dilute with high purity water; Again with filter sizes be the glass core filtration unit filtering and washing of 0.45 μm of micropore to pH=7, obtained filter cake, by gained filter cake dry 1-3 days at 50-70 DEG C, at being preferably 60 DEG C dry 2 days; In 950-1150 DEG C of calcination process 10-50s after being ground by filter cake again, be preferably 1100 DEG C of process 30s, i.e. obtained pretreating graphite powder;
Step 2, preparation graphene oxide solution
The pretreating graphite powder obtained with step one, for raw material, adopts traditional Hummer method first to prepare graphite oxide solution, and then obtains graphene oxide solution with ultrasonic stripping;
Step 3, preparation Fe (OH) 3colloid
At room temperature, according to 1 part of FeCl 36H 2o is dissolved in 1-8 part high purity water, preferably 5 parts of meters, by FeCl 36H 2o is dissolved in high purity water, obtains FeCl 3the aqueous solution; Again by FeCl 3the aqueous solution drops in the water of 30 parts of boilings, keeps the preferred 2min of solution boiling 1-4min, i.e. obtained Fe (OH) 3colloid;
Step 4, prepares macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite:
1. be preferably 2.0mg/mL by the graphene oxide solution that high purity water dilution step two is obtained to 1.0-4.0mg/mL, adjust its pH value with ammoniacal liquor and be preferably pH=9 to 8-10, obtained dilution graphene oxide solution;
2. at room temperature by Fe (OH) obtained for step 3 3colloid drops is added in 1. obtained dilution graphene oxide solution, control Fe (OH) 3be (0-3) with the mass ratio of dilution graphene oxide solution: 1 is preferably 1: 1, and stirs 0.5-3h and be preferably 1h, makes reaction solution;
3. 2. obtained reaction solution is moved in water heating kettle, under 150-220 DEG C of condition, leave standstill 15-30h, under being preferably 180 DEG C of conditions, leave standstill 24h, then water heating kettle is cooled to room temperature namely obtains Fe 2o 3@Graphene hydrogel;
4. by obtained Fe 2o 3it is in the ammoniacal liquor of 5-20% volume basis that@Graphene hydrogel moves in concentration, is preferably 10%, hydrothermal treatment consists 1-5h at 80-130 DEG C, hydrothermal treatment consists 3h at being preferably 120 DEG C;
5. the Fe processed in 4. 2o 3@Graphene hydrogel subzero 48 ~ subzero 58 DEG C, under pressure 5 ~ 30Pa condition, be preferably subzero 53 DEG C, pressure 10Pa, cold drying Fe 2o 3@graphene aerogel;
6. at 700-900 DEG C, 5. roasting obtains under High Purity Nitrogen atmospheric condition Fe 2o 3@graphene aerogel 3-8h, roasting 5h at being preferably 800 DEG C, obtains described macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite.
beneficial effect:
1, the present invention relates to a kind of macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite, mainly solves block Fe 3o 4surface area per unit volume amasss the problem that little and graphene-based material is easily reunited.In its preparation, the present invention adopts with FeCl 36H 2o is Fe (OH) prepared by raw material 3colloid is Fe 3o 4precursor, is added on and is raw material with pretreating graphite powder, in the graphene oxide solution that adopts traditional Hummer legal system standby, adopts hydrothermal reduction method to obtain in conjunction with ammoniacal liquor hydrothermal treatment consists and cold dry technology.Reaction conditions is relatively gentle, prepares fairly simple, is easy to realize relatively large production.
2, macroscopic three dimensional Fe provided by the present invention 3o 4@graphene aerogel ultra light composite, have concurrently simultaneously and improve the characteristic of Z 250 and graphene aerogel, can be used as organic dye sewage and adsorbent for heavy metal, super capacitor and electrode material of lithium battery, absorbing material, biotechnological formulation material etc.
Accompanying drawing explanation
Fig. 1 (a) and (b) are respectively Fe (OH) 3be 1: 1 and 1: 1.5 with graphene oxide feed ratio and in high pure nitrogen atmosphere 800 DEG C of roasting 5h gained Fe 3o 4the photo in kind of@graphene aerogel matrix material, can find out that obtained matrix material is macroscopical columnar three-dimensional structure;
Fig. 2 is made graphene oxide, graphene aerogel, Fe 2o 3and Fe (OH) 3be the Fe obtained under 1: 1 condition with graphene oxide feed ratio 2o 3@graphene aerogel and by 800 DEG C of roasting 5h gained Fe in its high pure nitrogen atmosphere 3o 4the XRD spectra of@graphene aerogel matrix material, therefrom can find out that graphene oxide is converted into Graphene by hydrothermal reduction process more up hill and dale, and Fe after pyroprocessing 2o 3be reduced to Fe 3o 4;
Fig. 3 (a) and (b) are respectively Fe (OH) 3with graphene oxide feed ratio be 1: 1,800 DEG C of roasting 5h gained Fe in high pure nitrogen atmosphere 3o 4the SEM photo of@graphene aerogel matrix material, can find out Fe 3o 4be scattered in graphene aerogel framework equably;
Fig. 4 is graphene aerogel and Fe (OH) 3with graphene oxide feed ratio be 1: 1,800 DEG C of roasting 5h gained Fe in high pure nitrogen atmosphere 3o 4the Raman spectrum of@graphene aerogel material, can find out that the introducing of iron species in hydrothermal reduction process does not obviously affect the reduction of graphene oxide;
Fig. 5 is Fe (OH) 3with graphene oxide feed ratio be 1: 1,800 DEG C of roasting 5h gained Fe in high pure nitrogen atmosphere 3o 4nitrogen adsorption-the desorption isotherm of@graphene aerogel matrix material at-196 DEG C and corresponding texture parameter (insertion), can find out that described matrix material all presents typical mesoporous material isotherm characteristic, mean pore size is about 5.00nm.
Embodiment
The present invention is set forth further below in conjunction with specific embodiment:
embodiment 1
Step one, pretreating graphite powder
Under room temperature, magnetic agitation condition, 35 g Graphite Powder 99s be added on the mix acid liquor (1: 3) of 520mL concentrated nitric acid and the vitriol oil and stir 24h.Add high purity water and be diluted to 1.5L, be that the glass core filtration unit filtering and washing of 0.45 μm of micropore is to neutral (pH=7) again with filter sizes, obtained filter cake, grinds gained filter cake after dry 2 days at 60 DEG C, and in batches in 1100 DEG C of process 30s i.e. obtained pretreating graphite powder.
Step 2, preparation graphene oxide solution
Make the pretreating graphite powder of acquisition for raw material with step one, adopt traditional Hummer legal system for graphite oxide solution, and then obtain graphene oxide solution with ultrasonic stripping, concentration is about 4.0mg/mL.
Step 3, prepares ferric hydroxide colloid
At room temperature, 1gFeCl 36H 2o is dissolved in 5mL high purity water, obtains FeCl 3the aqueous solution; Again by FeCl 3the aqueous solution drops in the water of 25mL boiling, keeps solution boiling 2min, i.e. obtained ferric hydroxide colloid; Concentration is about 33.3mg/mL.
Step 4, prepares macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite:
Fe (OH) 3be 0.5: 1 with graphene oxide mass ratio,
1. get the graphene oxide solution 15mL 15mL high purity water dilution that step 2 is obtained, then adjust its pH=9 with ammoniacal liquor under magnetic agitation, then supersound process 1h, obtained dilution graphene oxide solution;
2. at room temperature by 0.8mLFe (OH) obtained for step 3 3colloid drops is added in 1. obtained dilution graphene oxide solution, and stirs 1h and make reaction solution;
3. 2. obtained reaction solution is moved in 50mL water heating kettle, under 180 DEG C of conditions, leave standstill 24h; Then water heating kettle is cooled to room temperature and namely obtains Fe 2o 3@Graphene hydrogel;
4. the Fe will obtained 2o 3@Graphene hydrogel move in concentration be in the ammoniacal liquor of 10% volume basis, hydrothermal treatment consists 3h at 120 DEG C;
5. the Fe processed in 4. 2o 3@Graphene hydrogel subzero 53 DEG C, under pressure 10Pa condition, cold drying Fe 2o 3@graphene aerogel;
6. at 800 DEG C, 5. roasting obtains under High Purity Nitrogen atmospheric condition Fe 2o 3@graphene aerogel 5h, obtains described macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite matrix material.
embodiment 2
Step one to step 3 with embodiment 1.
Step 4, prepares macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite:
Fe (OH) 3be 1: 1 with the mass ratio of graphene oxide,
1. get the graphene oxide solution 15mL 15mL high purity water dilution that step 2 is obtained, then adjust its pH=9 with ammoniacal liquor under magnetic agitation, then supersound process 1h, obtained dilution graphene oxide solution;
2. at room temperature by 1.8mLFe (OH) obtained for step 3 3colloid drops is added in 1. obtained dilution graphene oxide solution, and stirs 1h and make reaction solution;
3. 2. obtained reaction solution is moved in 50mL water heating kettle, under 180 DEG C of conditions, leave standstill 24h; Then water heating kettle is cooled to room temperature and namely obtains Fe 2o 3@Graphene hydrogel;
4. the Fe will obtained 2o 3@Graphene hydrogel move in concentration be in the ammoniacal liquor of 10% volume basis, hydrothermal treatment consists 3h at 120 DEG C;
5. the Fe processed in 4. 2o 3@Graphene hydrogel subzero 53 DEG C, under pressure 10Pa condition, cold drying Fe 2o 3@graphene aerogel;
6. at 800 DEG C, 5. roasting obtains under High Purity Nitrogen atmospheric condition Fe 2o 3@graphene aerogel 5h, obtains described macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite matrix material.
embodiment 3
Step one to step 3 with embodiment 1.
Step 4, prepares macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite:
Fe (OH) 3be 1.5: 1 with the mass ratio of graphene oxide,
1. get the graphene oxide solution 15mL 15mL high purity water dilution that step 2 is obtained, then adjust its pH=9 with ammoniacal liquor under magnetic agitation, then supersound process 1h, obtained dilution graphene oxide solution;
2. at room temperature by 2.7mLFe (OH) obtained for step 3 3colloid drops is added in 1. obtained dilution graphene oxide solution, and stirs 1h;
3. 2. obtained reaction solution is moved in 50mL water heating kettle, under 180 DEG C of conditions, leave standstill 24h; Then water heating kettle is cooled to room temperature and namely obtains Fe 2o 3@Graphene hydrogel;
4. the Fe will obtained 2o 3@Graphene hydrogel move in concentration be in the ammoniacal liquor of 10% volume basis, hydrothermal treatment consists 3h at 120 DEG C;
5. the Fe processed in 4. 2o 3@Graphene hydrogel subzero 53 DEG C, under pressure 10Pa condition, cold drying Fe 2o 3@graphene aerogel;
6. at 800 DEG C, 5. roasting obtains under High Purity Nitrogen atmospheric condition Fe 2o 3@graphene aerogel 5h, obtains described macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite matrix material.
embodiment 4
Step one to step 3 with embodiment 1.
Step 4, prepares macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite:
Fe (OH) 3be 2: 1 with graphene oxide mass ratio,
1. get the graphene oxide solution 15mL 15mL high purity water dilution that step 2 is obtained, then adjust its pH=9 with ammoniacal liquor under magnetic agitation, then supersound process 1h, obtained dilution graphene oxide solution;
2. at room temperature by 3.6mLFe (OH) obtained for step 3 3colloid drops is added in 1. obtained dilution graphene oxide solution, and stirs 1h, makes reaction solution;
3. 2. obtained reaction solution is moved in 50mL water heating kettle, under 180 DEG C of conditions, leave standstill 24h; Then water heating kettle is cooled to room temperature and namely obtains Fe 2o 3@Graphene hydrogel,
4. the Fe will obtained 2o 3@Graphene hydrogel move in concentration be in the ammoniacal liquor of 10% volume basis, hydrothermal treatment consists 3h at 120 DEG C;
5. the Fe processed in 4. 2o 3@Graphene hydrogel subzero 53 DEG C, under pressure 10Pa condition, cold drying Fe 2o 3@graphene aerogel;
6. at 800 DEG C, 5. roasting obtains under High Purity Nitrogen atmospheric condition Fe 2o 3@graphene aerogel 5h, obtains described macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite matrix material.
embodiment 5
Step one to step 3 with embodiment 1.
Step 4, prepares macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite:
Fe (OH) 3be 2.5: 1 with graphene oxide mass ratio,
1. get the graphene oxide solution 15mL 15mL high purity water dilution that step 2 is obtained, then adjust its pH=9 with ammoniacal liquor under magnetic agitation, then supersound process 1h, obtained dilution graphene oxide solution;
2. at room temperature by 4.5mLFe (OH) obtained for step 3 3colloid drops is added in 1. obtained dilution graphene oxide solution, and stirs 1h;
3. 2. obtained reaction solution is moved in 50mL water heating kettle, under 180 DEG C of conditions, leave standstill 24h; Then water heating kettle is cooled to room temperature and namely obtains Fe 2o 3@Graphene hydrogel;
4. by obtained Fe 2o 3@Graphene hydrogel move in concentration be in the ammoniacal liquor of 10% volume basis, hydrothermal treatment consists 3h at 120 DEG C;
5. the Fe processed in 4. 2o 3@Graphene hydrogel subzero 53 DEG C, under pressure 10Pa condition, cold drying Fe 2o 3@graphene aerogel;
6. at 800 DEG C, 5. roasting obtains under High Purity Nitrogen atmospheric condition Fe 2o 3@graphene aerogel 5h, obtains described macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite matrix material.
embodiment 6
Step one is to step 3 embodiment 1.
Step 4, prepares macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite:
Fe (OH) 3be 3: 1 with graphene oxide mass ratio,
1. get the graphene oxide solution 15mL 15mL high purity water dilution that step 2 is obtained, then adjust its pH=9 with ammoniacal liquor under magnetic agitation, then supersound process 1h, obtained dilution graphene oxide solution;
2. at room temperature by 5.4mLFe (OH) obtained for step 3 3colloid drops is added in 1. obtained dilution graphene oxide solution, and stirs 1h, makes reaction solution;
3. 2. obtained reaction solution is moved in 50mL water heating kettle, under 180 DEG C of conditions, leave standstill 24h; Then water heating kettle is cooled to room temperature and namely obtains Fe 2o 3@Graphene hydrogel;
4. by obtained Fe 2o 3@Graphene hydrogel move in concentration be in the ammoniacal liquor of 10% volume basis, hydrothermal treatment consists 3h at 120 DEG C;
5. the Fe processed in 4. 2o 3@Graphene hydrogel subzero 53 DEG C, under pressure 10Pa condition, cold drying Fe 2o 3@graphene aerogel;
6. at 800 DEG C, 5. roasting obtains under High Purity Nitrogen atmospheric condition Fe 2o 3@graphene aerogel 5h, obtains described macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite matrix material.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.

Claims (4)

1. a macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite, is characterized in that: Fe by weight percentage 3o 4content be 0-65%, and be not 0%, Fe 3o 4content be preferably 25-55%, surplus is graphene aerogel.
2. a kind of macroscopic three dimensional Fe according to claim 1 3o 4@graphene aerogel ultra light composite, is characterized in that: density is 0.05-0.10g/cm 3, mean pore size is 3.00-7.00nm, total pore volume is 0.12-0.52cm 3/ g, specific surface area are 180-400m 2/ g.
3. a kind of macroscopic three dimensional Fe according to claim 1 3o 4@graphene aerogel ultra light composite, is characterized in that: a kind of macroscopic three dimensional Fe 3o 4the macroscopic three dimensional structure of@graphene aerogel ultra light composite is columnar structure, diameter 1-3cm, height 2-7cm.
4. a kind of macroscopic three dimensional Fe according to claim 1 3o 4@graphene aerogel ultra light composite, is characterized in that: preparation method comprises the following steps:
Step one, pretreating graphite powder:
First by concentrated nitric acid and the vitriol oil by volume 1: (1-5), be preferably 1: 3 and be mixed and made into mix acid liquor, at room temperature Graphite Powder 99 is put into mix acid liquor, (5-12) part Graphite Powder 99 is put into according to 100 parts of mix acid liquors, stir 16-32h, be preferably 100 parts of mix acid liquors and put into 10 parts of Graphite Powder 99s, stir 24h, then dilute with high purity water; Again with filter sizes be the glass core filtration unit filtering and washing of 0.45 μm of micropore to pH=7, obtained filter cake, by gained filter cake dry 1-3 days at 50-70 DEG C, at being preferably 60 DEG C dry 2 days; In 950-1150 DEG C of calcination process 10-50s after being ground by filter cake again, be preferably 1100 DEG C of process 30s, i.e. obtained pretreating graphite powder;
Step 2, preparation graphene oxide solution:
The pretreating graphite powder obtained with step one, for raw material, adopts traditional Hummer method first to prepare graphite oxide solution, and then obtains graphene oxide solution with ultrasonic stripping;
Step 3, preparation Fe (OH) 3colloid:
At room temperature, according to 1 part of FeCl 36H 2o is dissolved in 1-8 part high purity water, preferably 5 parts of meters, by FeCl 36H 2o is dissolved in high purity water, obtains FeCl 3the aqueous solution; Again by FeCl 3the aqueous solution drops in the water of 30 parts of boilings, keeps the preferred 2min of solution boiling 1-4min, i.e. obtained Fe (OH) 3colloid;
Step 4, prepares macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite:
1. be preferably 2.0mg/mL by the graphene oxide solution that high purity water dilution step two is obtained to 1.0-4.0mg/mL, then adjust its pH value with ammoniacal liquor and be preferably pH=9 to 8-10, obtainedly dilute graphene oxide solution;
2. at room temperature by Fe (OH) obtained for step 3 3colloid drops is added in 1. obtained dilution graphene oxide solution, control Fe (OH) 3be (0-3) with the mass ratio of dilution graphene oxide solution: 1 is preferably 1: 1, and stirs 0.5-3h and be preferably 1h, makes reaction solution;
3. 2. obtained reaction solution is moved in water heating kettle, under 150-220 DEG C of condition, leave standstill 15-30h, under being preferably 180 DEG C of conditions, leave standstill 24h, then water heating kettle is cooled to room temperature namely obtains Fe 2o 3@Graphene hydrogel;
4. by obtained Fe 2o 3it is in the ammoniacal liquor of 5-20% volume basis that@Graphene hydrogel moves in concentration, is preferably 10%, hydrothermal treatment consists 1-5h at 80-130 DEG C, hydrothermal treatment consists 3h at being preferably 120 DEG C;
5. the Fe processed in 4. 2o 3@Graphene hydrogel subzero 48 ~ subzero 58 DEG C, under pressure 5 ~ 30Pa condition, be preferably subzero 53 DEG C, pressure 10Pa, cold drying Fe 2o 3@graphene aerogel;
6. at 700-900 DEG C, 5. roasting obtains under High Purity Nitrogen atmospheric condition Fe 2o 3@graphene aerogel 3-8h, roasting 5h at being preferably 800 DEG C, obtains described macroscopic three dimensional Fe 3o 4@graphene aerogel ultra light composite.
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