CN103723705A - Graphene/nano-aluminum compound and preparation method thereof - Google Patents
Graphene/nano-aluminum compound and preparation method thereof Download PDFInfo
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- CN103723705A CN103723705A CN201210388903.2A CN201210388903A CN103723705A CN 103723705 A CN103723705 A CN 103723705A CN 201210388903 A CN201210388903 A CN 201210388903A CN 103723705 A CN103723705 A CN 103723705A
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Abstract
The invention discloses a graphene/nano-aluminum compound and a preparation method thereof. The method comprises the following steps: dispersing graphite oxide in an NaHCO3 solution to prepare a graphite oxide dispersion, carrying out ultrasonic treatment, adding Al2(SO4)3 while stirring with a mass ratio of Al2(SO4)3 to the graphite oxide of 0.79-2.11:1, filtering, collecting a coarse filtration material, washing, and drying to obtain a graphene oxide/aluminum hydroxide compound; and carrying out reduction treatment of the graphene oxide/aluminum hydroxide compound in weak reduction atmosphere, calcining under the protection of an inert gas, cooling, and grinding to obtain the graphene/nano-aluminum compound with the mass percentage content of graphene of 60-80%. The graphene/nano-aluminum compound prepared in the invention has the advantages of few defects, high mass percentage content of graphene, good conductivity, and effective overcome of the mass agglomeration of graphene after the reduction. The preparation method has the advantages of simplicity, feasibility and low cost.
Description
Technical field
The invention belongs to material chemistry technical field, be specifically related to a kind of graphene/nanometer aluminium mixture and preparation method thereof.
Background technology
Graphene is a kind of monolayer carbon atomic plane material separating from graphite, it is current the thinnest material in the world, its special structure makes it have the advantages such as high surface area, high conductivity, high mechanical strength and excellent toughness, therefore, in a lot of fields, there is the potential of application, the preparation of grapheme material study hotspot especially.At present, Graphene can be prepared by methods such as electrochemical process, chemical Vapor deposition process, micromechanics stripping methods, but easily produces Graphene agglomeration, and the generation of this phenomenon also can reduce the specific surface area of Graphene, thereby affects the performance of Graphene.
For Graphene agglomeration, in prior art, recorded inorganic nano material has been dispersed in to the method for preparing Graphene/inorganic nano material mixture in Graphene surface to solve this difficult problem, but these method effects are not ideal enough and the mixture prepared in Graphene content lower, directly cause the specific conductivity of the mixture of preparing lower, greatly limited researchdevelopment and the application of Graphene.
Summary of the invention
For addressing the above problem, the present invention aims to provide a kind of preparation method of graphene/nanometer aluminium mixture, the method can prepare Graphene quality percentage composition higher, the good graphene/nanometer aluminium of conductivity mixture, and can effectively overcome a large amount of reunions of Graphene after reduction.
The preparation method of a kind of graphene/nanometer aluminium mixture provided by the invention, is characterized in that, comprises the following steps: graphite oxide is dispersed in to NaHCO
3in solution, make graphite oxide dispersion liquid, ultrasonic, by Al
2(SO
4)
3with the mass ratio of graphite oxide be that 0.79 ~ 2.11:1 stirs and adds Al
2(SO
4)
3, filter, collect colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; Described graphene oxide/aluminium hydroxide mixture is placed in to reduction under weakly reducing atmosphere to be processed; and then calcine under protection of inert gas; cooling, grind and obtain graphene/nanometer aluminium mixture, in described graphene/nanometer aluminium mixture, the quality percentage composition of Graphene is 60 ~ 80%.
Preferably, Al
2(SO
4)
3with the mass ratio of graphite oxide be 1.06 ~ 1.70:1.More preferably, Al
2(SO
4)
3with the mass ratio of graphite oxide be 1.36:1.
Preferably, the preparation method of graphite oxide is: the graphite that is 99.5% by purity adds in the vitriol oil, then adds potassium permanganate to form mixture, and the temperature of mixture is remained between 0 ~ 10 ℃ and stirs 2 ~ 4h, mixture is stirred to 12 ~ 24h in room-temperature water bath, under condition of ice bath, in mixture, slowly add deionized water, graphite is oxidized, and add hydrogen peroxide to remove potassium permanganate in mixture, suction filtration, solids is carried out to repetitive scrubbing with dilute hydrochloric acid, dry, obtain graphite oxide; The mass ratio of described graphite and described potassium permanganate is 1:1.5 ~ 5, and the solid-to-liquid ratio of described graphite and the described vitriol oil is 1 ~ 5g:20 ~ 50ml, and the mass ratio of described hydrogen peroxide and described potassium permanganate is 0.5:1.
Preferably, NaHCO
3the concentration of solution is 0.1 ~ 1.2mol/L.
Preferably, the concentration of graphite oxide dispersion liquid is 5 ~ 15g/L.More preferably, the concentration of graphite oxide dispersion liquid is 3 ~ 7g/L.
Preferably, weakly reducing atmosphere is that volume ratio is the nitrogen of 95:5 and the gas mixture of hydrogen, the volume ratio argon gas that is 10:1 ~ 0.5 and the gas mixture of hydrogen.
Preferably, when reduction is processed, reduction temperature is 150 ~ 300 ℃, and the recovery time is 1 ~ 2 hour
Preferably, rare gas element is argon gas, and the temperature of calcining is 600 ~ 800 ℃.
Preferably, the specific surface area of graphene/nanometer aluminium mixture is 200 ~ 800m
2/ g.
And, the graphene/nanometer aluminium mixture that the present invention also provides aforesaid method to make.
Compared with prior art, a kind of graphene/nanometer aluminium mixture provided by the invention and preparation method thereof has following beneficial effect:
The present invention adopts method redox graphene/aluminium hydroxide mixture of thermal reduction, functional group's (as hydroxyl, carbonyl etc.) to graphene oxide at higher temperature reduces, the defect that Graphene is produced is less, in the graphene/nanometer aluminium mixture obtaining, the quality percentage composition of Graphene is higher, the density of Graphene in matrix is increased, increase the path of conduction, therefore increased the electroconductibility of graphene/nanometer aluminium mixture.And, in the process of preparing Graphene, prepare nano aluminum particle simultaneously, adopt nano aluminum particle to be distributed to Graphene surface and obtain graphene/nanometer aluminium mixture, the existence of nano aluminum has increased the distance between graphene sheet layer, thereby reduce interaction therebetween, solved the agglomeration that Graphene too high levels easily causes.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the scanning electron microscope diagram of the graphene/nanometer aluminium mixture that makes of the embodiment of the present invention 1.
Fig. 2 is the adsorption-desorption isothermal curve figure of the graphene/nanometer aluminium mixture that makes of the embodiment of the present invention 1.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The preparation method of a kind of graphene/nanometer aluminium mixture provided by the invention, is characterized in that, comprises the following steps: graphite oxide is dispersed in to NaHCO
3in solution, make graphite oxide dispersion liquid, ultrasonic, by Al
2(SO
4)
3with the mass ratio of graphite oxide be that 0.79 ~ 2.11:1 stirs and adds Al
2(SO
4)
3, filter, collect colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; Described graphene oxide/aluminium hydroxide mixture is placed in to reduction under weakly reducing atmosphere to be processed; and then calcine under protection of inert gas; cooling, grind and obtain graphene/nanometer aluminium mixture, in described graphene/nanometer aluminium mixture, the quality percentage composition of Graphene is 60 ~ 80%.
Al
2(SO
4)
3with the mass ratio of graphite oxide be 1.06 ~ 1.70:1.Al
2(SO
4)
3with the mass ratio of graphite oxide be 1.36:1.
The preparation method of graphite oxide is: the graphite that is 99.5% by purity adds in the vitriol oil, then add potassium permanganate to form mixture, the temperature of mixture is remained between 0 ~ 10 ℃ and stirs 2 ~ 4h, mixture is stirred to 12 ~ 24h in room-temperature water bath, under condition of ice bath, in mixture, slowly add deionized water, graphite is oxidized, and adding hydrogen peroxide to remove potassium permanganate in mixture, suction filtration, carries out repetitive scrubbing to solids with dilute hydrochloric acid, dry, obtain graphite oxide; The mass ratio of described graphite and described potassium permanganate is 1:1.5 ~ 5, and the solid-to-liquid ratio of described graphite and the described vitriol oil is 1 ~ 5g:20 ~ 50ml, and the mass ratio of described hydrogen peroxide and described potassium permanganate is 0.5:1.
NaHCO
3the concentration of solution is 0.1 ~ 1.2mol/L.
The concentration of graphite oxide dispersion liquid is 5 ~ 15g/L.The concentration of graphite oxide dispersion liquid is 3 ~ 7g/L.
Ultrasonic condition is ultrasonic 2 hours of 200W.
Weakly reducing atmosphere is the gas mixture of gas mixture, argon gas and the hydrogen of nitrogen and hydrogen.In the gas mixture of nitrogen and hydrogen, the volume ratio of nitrogen and hydrogen is 95:5.In the gas mixture of argon gas and hydrogen, the volume ratio of argon gas and hydrogen is 10:1 ~ 0.5.
When reduction is processed, reduction temperature is 150 ~ 300 ℃, and the recovery time is 1 ~ 2 hour
Rare gas element is argon gas, and the temperature of calcining is 600 ~ 800 ℃.
The specific surface area of graphene/nanometer aluminium mixture is 200 ~ 800m
2/ g.
And, the invention provides the graphene/nanometer aluminium mixture being made by above-mentioned steps.
Compared with prior art, a kind of graphene/nanometer aluminium mixture provided by the invention and preparation method thereof has following beneficial effect:
The present invention adopts method redox graphene/aluminium hydroxide mixture of thermal reduction, functional group's (as hydroxyl, carbonyl etc.) to graphene oxide at higher temperature reduces, the defect that Graphene is produced is less, in the graphene/nanometer aluminium mixture obtaining, the quality percentage composition of Graphene is higher, the density of Graphene in matrix is increased, increase the path of conduction, therefore increased the electroconductibility of graphene/nanometer aluminium mixture.And, in the process of preparing Graphene, prepare nano aluminum particle simultaneously, adopt nano aluminum particle to be distributed to Graphene surface and obtain graphene/nanometer aluminium mixture, the existence of nano aluminum has increased the distance between graphene sheet layer, thereby reduce interaction therebetween, solved the agglomeration that Graphene too high levels easily causes.
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Embodiment 1
Take the graphite of 10g purity 99.5%, adding 350mL massfraction is in 98% the vitriol oil, then adds 40g potassium permanganate to be oxidized, and this mixing solutions is remained on to 4 ℃, stirs 4h, then in room-temperature water bath, stirs 18h.Then under condition of ice bath, slowly add deionized water.After 15min, then add 20g hydrogen peroxide to remove potassium permanganate, mixture color becomes glassy yellow afterwards, suction filtration, then the dilute hydrochloric acid that is 10% by 5L concentration washing 3 times, suction filtration, at 60 ℃ of vacuum-drying 48h, obtain graphite oxide.Get the graphite oxide that 2.7g obtains and be dispersed in the NaHCO that 550mL concentration is 0.1mol/L
3in solution, make the dispersion liquid that graphite oxide concentration is 5g/L, ultrasonic 2 hours of 200W, stirs and adds 0.01mol Al
2(SO
4)
3, filter, collect colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to the lower 150 ℃ of reduction of gas mixture (volume ratio 95:5) atmosphere of nitrogen and hydrogen 1 hour, then under argon atmosphere 300 ℃ calcining 3 hours, cooling, grind and obtain the graphene/nanometer aluminium mixture that Graphene quality percentage composition is 70%.
The scanning electron microscope diagram of gained graphene/nanometer aluminium mixture as shown in Figure 1, can be known and see graphene film and nano particle, be evenly distributed.
As shown in Figure 2, specific surface area is 275m to the adsorption-desorption isothermal curve figure of gained graphene/nanometer aluminium mixture as seen from the figure
2/ g.
Embodiment 2
Take the graphite of 10g purity 99.5%, adding 100mL massfraction is in 98% the vitriol oil, then adds 50g potassium permanganate to be oxidized, and this mixing solutions is remained on to 10 ℃, stirs 2h, then in room-temperature water bath, stirs 12h.Then under condition of ice bath, slowly add deionized water.After 15min, then add 25g hydrogen peroxide to remove potassium permanganate, mixture color becomes glassy yellow afterwards, suction filtration, then the dilute hydrochloric acid that is 10% by 5L concentration washing 3 times, suction filtration, at 60 ℃ of vacuum-drying 48h, obtain graphite oxide.Get the graphite oxide that 7.2g obtains and be dispersed in the NaHCO that 900mL concentration is 0.3mol/L
3in solution, make the dispersion liquid that graphite oxide concentration is 8g/L, ultrasonic 2 hours of 200W, stirs and adds 0.02mol Al
2(SO
4)
3, filter, collect colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to the lower 300 ℃ of reductase 12s hour of gas mixture (volume ratio 10:0.5) atmosphere of argon gas and hydrogen, then under atmosphere of inert gases 600 ℃ calcining 6 hours, cooling, grind and obtain the graphene/nanometer aluminium mixture that Graphene quality percentage composition is 80%.
Embodiment 3
Take the graphite of 30g purity 99.5%, adding 120mL massfraction is in 98% the vitriol oil, then adds 45g potassium permanganate to be oxidized, and this mixing solutions is remained on to 8 ℃, stirs 3h, then in room-temperature water bath, stirs 20h.Then under condition of ice bath, slowly add deionized water.After 15min, then add 22.5g hydrogen peroxide to remove potassium permanganate, mixture color becomes glassy yellow afterwards, suction filtration, then the dilute hydrochloric acid that is 10% by 5L concentration washing 3 times, suction filtration, at 60 ℃ of vacuum-drying 48h, obtain graphite oxide.Get the graphite oxide that 10.8g obtains and be dispersed in the NaHCO that 1100mL concentration is 0.8mol/L
3in solution, make the dispersion liquid that graphite oxide concentration is 10g/L, ultrasonic 2 hours of 200W, stirs and adds 0.03mol Al
2(SO
4)
3, filter, collect colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to the lower 300 ℃ of reductase 12s hour of gas mixture (volume ratio 10:1) atmosphere of argon gas and hydrogen, then under argon atmosphere 600 ℃ calcining 3 hours, cooling, grind and obtain the graphene/nanometer aluminium mixture that Graphene quality percentage composition is 75%.
Embodiment 4
Take the graphite of 20g purity 99.5%, adding 180mL massfraction is in 98% the vitriol oil, then adds 60g potassium permanganate to be oxidized, and this mixing solutions is remained on to 0 ℃, stirs 4h, then in room-temperature water bath, stirs 24h.Then under condition of ice bath, slowly add deionized water.After 15min, then add 30g hydrogen peroxide to remove potassium permanganate, mixture color becomes glassy yellow afterwards, suction filtration, then the dilute hydrochloric acid that is 10% by 5L concentration washing 3 times, suction filtration, at 60 ℃ of vacuum-drying 48h, obtain graphite oxide.Get the graphite oxide that 13.2g obtains and be dispersed in the NaHCO that 1000mL concentration is 1.2mol/L
3in solution, make the dispersion liquid that graphite oxide concentration is 13g/L, ultrasonic 2 hours of 200W, stirs and adds 0.06mol Al
2(SO
4)
3, filter, collect colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to the lower 300 ℃ of reduction of gas mixture (volume ratio 10:0.5) atmosphere of argon gas and hydrogen 1 hour, then under argon atmosphere 600 ℃ calcining 6 hours, cooling, grind and obtain the graphene/nanometer aluminium mixture that Graphene quality percentage composition is 65%.
Embodiment 5
Take the graphite of 20g purity 99.5%, adding 400mL massfraction is in 98% the vitriol oil, then adds 80g potassium permanganate to be oxidized, and this mixing solutions is remained on to 0 ℃, stirs 2h, then in room-temperature water bath, stirs 24h.Then under condition of ice bath, slowly add deionized water.After 15min, then add 40g hydrogen peroxide to remove potassium permanganate, mixture color becomes glassy yellow afterwards, suction filtration, then the dilute hydrochloric acid that is 10% by 5L concentration washing 3 times, suction filtration, at 60 ℃ of vacuum-drying 48h, obtain graphite oxide.Get the graphite oxide that 16.2g obtains and be dispersed in the NaHCO that 1100mL concentration is 0.3mol/L
3in solution, make the dispersion liquid that graphite oxide concentration is 15g/L, ultrasonic 2 hours of 200W, stirs and adds 0.1mol Al
2(SO
4)
3, filter, collect colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to the lower 300 ℃ of reductase 12s hour of gas mixture (volume ratio 10:0.5) atmosphere of argon gas and hydrogen, then under atmosphere of inert gases 600 ℃ calcining 6 hours, cooling, grind and obtain the graphene/nanometer aluminium mixture that Graphene quality percentage composition is 60%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. a graphene/nanometer aluminium mixture preparation method, is characterized in that, comprises the following steps: graphite oxide is dispersed in to NaHCO
3in solution, make graphite oxide dispersion liquid, ultrasonic, by Al
2(SO
4)
3with the mass ratio of graphite oxide be that 0.79 ~ 2.11:1 stirs and adds Al
2(SO
4)
3, filter, collect colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; Described graphene oxide/aluminium hydroxide mixture is placed in to reduction under weakly reducing atmosphere to be processed; and then calcine under protection of inert gas; cooling, grind and obtain graphene/nanometer aluminium mixture, in described graphene/nanometer aluminium mixture, the quality percentage composition of Graphene is 60 ~ 80%.
2. graphene/nanometer aluminium mixture preparation method as claimed in claim 1, it is characterized in that, the preparation method of described graphite oxide is: the graphite that is 99.5% by purity adds in the vitriol oil, then add potassium permanganate to form mixture, the temperature of mixture is remained between 0 ~ 10 ℃ and stirs 2 ~ 4h, mixture is stirred to 12 ~ 24h in room-temperature water bath, under condition of ice bath, in mixture, slowly add deionized water, graphite is oxidized, and add hydrogen peroxide to remove potassium permanganate in mixture, suction filtration, solids is carried out to repetitive scrubbing with dilute hydrochloric acid, dry, obtain graphite oxide, the mass ratio of described graphite and described potassium permanganate is 1:1.5 ~ 5, and the solid-to-liquid ratio of described graphite and the described vitriol oil is 1 ~ 5g:20 ~ 50ml, and the mass ratio of described hydrogen peroxide and described potassium permanganate is 0.5:1.
3. graphene/nanometer aluminium mixture preparation method as claimed in claim 1, is characterized in that described NaHCO
3the concentration of solution is 0.1 ~ 1.2mol/L.
4. graphene/nanometer aluminium mixture preparation method as claimed in claim 1, is characterized in that, the concentration of described graphite oxide dispersion liquid is 5 ~ 15g/L.
5. graphene/nanometer aluminium mixture preparation method as claimed in claim 1, is characterized in that, it is the nitrogen of 95:5 and the gas mixture of hydrogen, the volume ratio argon gas that is 10:1 ~ 0.5 and the gas mixture of hydrogen that described weakly reducing atmosphere is selected from volume ratio.
6. graphene/nanometer aluminium mixture preparation method as claimed in claim 1, is characterized in that, when described reduction is processed, reduction temperature is 150 ~ 300 ℃, and the recovery time is 1 ~ 2 hour.
7. graphene/nanometer aluminium mixture preparation method as claimed in claim 1, is characterized in that, described rare gas element is argon gas, and the temperature of described calcining is 600 ~ 800 ℃.
8. graphene/nanometer aluminium mixture preparation method as claimed in claim 1, is characterized in that, the specific surface area of described graphene/nanometer aluminium mixture is 200 ~ 800m
2/ g.
9. a graphene/nanometer aluminium mixture, is characterized in that: described graphene/nanometer aluminium mixture is by the method preparation described in 1 ~ 8 arbitrary claim.
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