CN103723704A - Graphene/nano-alumina compound and preparation method thereof - Google Patents
Graphene/nano-alumina compound and preparation method thereof Download PDFInfo
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- CN103723704A CN103723704A CN201210388901.3A CN201210388901A CN103723704A CN 103723704 A CN103723704 A CN 103723704A CN 201210388901 A CN201210388901 A CN 201210388901A CN 103723704 A CN103723704 A CN 103723704A
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Abstract
The invention discloses a graphene/nano-alumina compound and a preparation method thereof. The method comprises the following steps: mixing block Al2(SO4)3 with graphite oxide with a mass ratio of 1.12-2.51:1, carrying out ball milling for 5-10h, adding ammonia water with the mass fraction of 5-10% having an amount 30-100% higher than a stoichiometric proportion for gradual generation of a precipitate, stirring for 1-4h until the amount of the precipitation no longer increases, allowing the obtained mixture to stand for 24h, filtering, collecting a coarse filtration material, washing, and drying to obtain a graphene oxide/aluminum hydroxide compound; and calcining the graphene oxide/aluminum hydroxide compound in protective gas atmosphere, cooling, and grinding to obtain the graphene/nano-alumina compound with the mass percentage content of graphene of 40-60%. The graphene/nano-alumina compound prepared in the invention has the advantages of uniform particle, high mass percentage of graphene, and good conductivity. 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 alumina compound 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 high surface area, high conductivity, high mechanical strength and the excellent advantages such as toughness, therefore, the potential that has application in a lot of fields, the preparation of grapheme material is 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 by inorganic nano material be dispersed in prepare Graphene/inorganic nano material mixture in Graphene surface method 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 prepared 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 alumina compound, the method can effectively overcome a large amount of reunions of Graphene after reduction, and then can obtain high specific surface area, and can prepare Graphene quality percentage composition higher, the good graphene/nanometer alumina compound of conductivity.
The preparation method of a kind of graphene/nanometer alumina compound provided by the invention, is characterized in that, comprises the following steps: by block Al
2(SO
4)
3with graphite oxide in mass ratio 1.12 ~ 2.51: 1 mixes, ball milling 5 ~ 10h, by stoichiometric ratio excessive 30%～100%, adding massfraction is again 5 ~ 10% ammoniacal liquor, has gradually precipitation to generate, and stirs 1 ~ 4h, until precipitation no longer increases, standing 24h, filters, and collects colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; Described graphene oxide/aluminium hydroxide mixture is calcined under protective gas atmosphere, cooling, grind and obtain graphene/nanometer alumina compound, in described graphene/nanometer alumina compound, the quality percentage composition of Graphene is 40 ~ 60%.
Preferably, Al
2(SO
4)
3with the mass ratio of graphite oxide be 1.37 ~ 2.05:1.More preferably, Al
2(SO
4)
3with the mass ratio of graphite oxide be 1.68:1.
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, with dilute hydrochloric acid, solids is carried out to repetitive scrubbing, 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, protective gas is selected from ammonia, nitrogen, argon gas, BH
3in one or more mixture.
Preferably, the temperature of calcining is 600 ~ 800 ℃.
Preferably, the specific surface area of graphene/nanometer alumina compound is 200 ~ 800m
2/ g.
And, the graphene/nanometer alumina compound that the present invention also provides aforesaid method to make.
Compared with prior art, a kind of graphene/nanometer alumina compound provided by the invention and preparation method thereof has following beneficial effect:
The present invention is prepared in graphene/nanometer alumina compound process, Tai-Ace S 150 and graphite oxide are mixed also to fully ball milling, can obtain the particle of uniform particle diameter, the graphene/nanometer alumina compound finally obtaining has excellent surface property, while being applied in battery, be not easy dry linting, extending battery life, and in the present invention, graphene oxide/aluminium hydroxide mixture is not directly placed under protective gas atmosphere and calcines through reduction step, can remove the oxygen on graphene oxide, and reduzate still leaves partial function group, make the graphene sheet layer after reduction can rely on each other electrostatic repulsion forces to reach good dispersion effect, and in preparing the process of Graphene, prepare nano alumina particles simultaneously, adopt nano alumina particles to be distributed to Graphene surface and obtain graphene/nanometer alumina compound, the existence of nano aluminium oxide has increased the distance between graphene sheet layer, prevent Graphene reunion, produce high specific surface area, secondly, in graphene/nanometer alumina compound of the present invention, Graphene is when reunion degree is lower, and the quality percentage composition of Graphene is higher, and the density of Graphene in matrix is increased, increase the path of conduction, therefore increased the electroconductibility of graphene/nanometer alumina compound.
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 alumina compound that makes of the embodiment of the present invention 1.
Fig. 2 is the adsorption-desorption isothermal curve figure of the graphene/nanometer alumina compound 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 alumina compound provided by the invention, is characterized in that, comprises the following steps: by block Al
2(SO
4)
3with graphite oxide in mass ratio 1.12 ~ 2.51: 1 mixes, ball milling 5 ~ 10h, by stoichiometric ratio excessive 30% ~ 100%, adding massfraction is again 5 ~ 10% ammoniacal liquor, has gradually precipitation to generate, and stirs 1 ~ 4h, until precipitation no longer increases, standing 24h, filters, and collects colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; Described graphene oxide/aluminium hydroxide mixture is calcined under protective gas atmosphere, cooling, grind and obtain graphene/nanometer alumina compound, in described graphene/nanometer alumina compound, the quality percentage composition of Graphene is 40 ~ 60%.
Al
2(SO
4)
3with the mass ratio of graphite oxide be 1.37 ~ 2.05:1.Al
2(SO
4)
3with the mass ratio of graphite oxide be 1.68:1.
The preparation method of graphite oxide is: the graphite that just purity is 99.5% 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 with dilute hydrochloric acid to solids, 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.
Protective gas is selected from ammonia, nitrogen, argon gas, BH
3in one or more mixture.
The temperature of calcining is 600 ~ 800 ℃.
The specific surface area of graphene/nanometer alumina compound is 200 ~ 800m
2/ g.
And, the graphene/nanometer alumina compound that the present invention also provides aforesaid method to make.
Compared with prior art, a kind of graphene/nanometer alumina compound provided by the invention and preparation method thereof has following beneficial effect:
The present invention is prepared in graphene/nanometer alumina compound process, Tai-Ace S 150 and graphite oxide are mixed also to fully ball milling, can obtain the particle of uniform particle diameter, the graphene/nanometer alumina compound finally obtaining has excellent surface property, while being applied in battery, be not easy dry linting, extending battery life, and in the present invention, graphene oxide/aluminium hydroxide mixture is not directly placed under protective gas atmosphere and calcines through reduction step, can remove the oxygen on graphene oxide, and reduzate still leaves partial function group, make the graphene sheet layer after reduction can rely on each other electrostatic repulsion forces to reach good dispersion effect, and in preparing the process of Graphene, prepare nano alumina particles simultaneously, adopt nano alumina particles to be distributed to Graphene surface and obtain graphene/nanometer alumina compound, the existence of nano aluminium oxide has increased the distance between graphene sheet layer, prevent Graphene reunion, produce high specific surface area, secondly, in graphene/nanometer alumina compound of the present invention, Graphene is when reunion degree is lower, and the quality percentage composition of Graphene is higher, and the density of Graphene in matrix is increased, increase the path of conduction, therefore increased the electroconductibility of graphene/nanometer alumina compound.
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 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.Take the graphite oxide that 8.2g obtains, with 13.7g Al
2(SO
4)
3mix, ball milling 5h, then by stoichiometric ratio excessive 30%, to add massfraction be 5% ammoniacal liquor, stirs 1h, standing 24h, filters, and collects colature washing, dry, obtains graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to 800 degree calcinings under argon atmosphere, cooling, the graphene/nanometer alumina compound that the quality percentage composition that obtains Graphene after taking-up grinding is 50%.
The scanning electron microscope diagram of gained graphene/nanometer alumina compound 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 alumina compound as seen from the figure
2/ g.
Embodiment 2
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.Take the graphite oxide that 3.1g obtains, with 3.4gAl
2(SO
4)
3mix, ball milling 8h, then by stoichiometric ratio excessive 50%, to add massfraction be 8% ammoniacal liquor, stirs 2h, standing 24h, filters, and collects colature washing, dry, obtains graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to 800 degree calcinings under ammonia/nitrogen atmosphere, cooling, nitrogen-doped graphene/nano aluminium oxide mixture that the quality percentage composition that obtains Graphene after taking-up grinding is 60%.
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.Take the graphite oxide that 1.7g obtains, with 2.4g Al
2(SO
4)
3mix, ball milling 10h, then by stoichiometric ratio excessive 80%, to add massfraction be 10% ammoniacal liquor, stirs 3h, standing 24h, filters, and collects colature washing, dry, obtains graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to BH
3under/nitrogen atmosphere, 600 degree calcinings, cooling, boron doped graphene/nano aluminium oxide mixture that the quality percentage composition that obtains Graphene after taking-up grinding is 55%.
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.Take the graphite oxide that 2g obtains, with 5.1gAl
2(SO
4)
3mix, ball milling 9h, then by stoichiometric ratio excessive 100%, to add massfraction be 10% ammoniacal liquor, stirs 4h, standing 24h, filters, and collects colature washing, dry, obtains graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to 600 degree calcinings under hydrogen/nitrogen atmosphere, cooling, the graphene/nanometer alumina compound that the quality percentage composition that obtains Graphene after taking-up grinding is 40%.
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.Take the graphite oxide that 1.4g obtains, with 2.7g Al
2(SO
4)
3mix, ball milling 5h, then by stoichiometric ratio excessive 50%, to add massfraction be 5% ammoniacal liquor, stirs 2h, standing 24h, filters, and collects colature washing, dry, obtains graphene oxide/aluminium hydroxide mixture; This graphene oxide/aluminium hydroxide mixture is placed in to 600 degree calcinings under hydrogen/nitrogen atmosphere, cooling, the graphene/nanometer alumina compound that the quality percentage composition that obtains Graphene after taking-up grinding is 45%.
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 (6)
1. a graphene/nanometer alumina compound preparation method, is characterized in that, comprises the following steps: by block Al
2(SO
4)
3with graphite oxide in mass ratio 1.12 ~ 2.51: 1 mixes, ball milling 5 ~ 10h, by stoichiometric ratio excessive 30% ~ 100%, adding massfraction is again 5 ~ 10% ammoniacal liquor, has gradually precipitation to generate, and stirs 1 ~ 4h, until precipitation no longer increases, standing 24h, filters, and collects colature washing, dry, obtain graphene oxide/aluminium hydroxide mixture; Described graphene oxide/aluminium hydroxide mixture is calcined under protective gas atmosphere, cooling, grind and obtain graphene/nanometer alumina compound, in described graphene/nanometer alumina compound, the quality percentage composition of Graphene is 40 ~ 60%.
2. graphene/nanometer alumina compound 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, with dilute hydrochloric acid, solids is carried out to repetitive scrubbing, 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 alumina compound preparation method as claimed in claim 1, is characterized in that, described protective gas is selected from ammonia, nitrogen, argon gas, BH
3in one or more mixture.
4. graphene/nanometer alumina compound preparation method as claimed in claim 1, is characterized in that, the temperature of described calcining is 600 ~ 800 ℃.
5. graphene/nanometer alumina compound preparation method as claimed in claim 1, is characterized in that, the specific surface area of described graphene/nanometer alumina compound is 200 ~ 800m
2/ g.
6. a graphene/nanometer alumina compound, is characterized in that: described graphene/nanometer alumina compound is by the method preparation described in 1 ~ 5 arbitrary claim.
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| CN104877169A (en) * | 2015-05-27 | 2015-09-02 | 河北大学 | Preparation method and application of inorganic hybrid flame retardant with high thermal stability |
| CN105542906A (en) * | 2015-12-03 | 2016-05-04 | 高大元 | Preparation method of metal anti-wear agent |
| CN106634863A (en) * | 2016-12-30 | 2017-05-10 | 深圳市大族元亨光电股份有限公司 | Graphene based silica gel heat-conductive gasket and preparation method thereof |
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| CN102153077A (en) * | 2011-05-12 | 2011-08-17 | 北京工业大学 | Method for preparing single-layer graphene with high carbon-oxygen ratio |
| CN102602917A (en) * | 2012-03-19 | 2012-07-25 | 华南理工大学 | Preparation method of nitrogen doped graphene/ metal oxide nanometer composite material |
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2012
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Patent Citations (2)
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| CN102153077A (en) * | 2011-05-12 | 2011-08-17 | 北京工业大学 | Method for preparing single-layer graphene with high carbon-oxygen ratio |
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| CN104877169A (en) * | 2015-05-27 | 2015-09-02 | 河北大学 | Preparation method and application of inorganic hybrid flame retardant with high thermal stability |
| CN105542906A (en) * | 2015-12-03 | 2016-05-04 | 高大元 | Preparation method of metal anti-wear agent |
| CN106634863A (en) * | 2016-12-30 | 2017-05-10 | 深圳市大族元亨光电股份有限公司 | Graphene based silica gel heat-conductive gasket and preparation method thereof |
| CN108530954A (en) * | 2018-04-10 | 2018-09-14 | 宁波工程学院 | A kind of preparation method of graphene coated aluminium hydrate nano composite material |
| CN109503888A (en) * | 2018-11-28 | 2019-03-22 | 沈阳理工大学 | A kind of preparation method of boehmite/graphene composite material |
| CN109503888B (en) * | 2018-11-28 | 2020-09-08 | 沈阳理工大学 | Preparation method of boehmite/graphene composite material |
| CN110143587A (en) * | 2019-05-27 | 2019-08-20 | 西安交通大学 | A method of so that graphene uniform is loaded micro-and nano-particles |
| CN110819222A (en) * | 2019-11-22 | 2020-02-21 | 安徽新大陆特种涂料有限责任公司 | Preparation method of anticorrosive antistatic machine tool coating |
| CN110819222B (en) * | 2019-11-22 | 2021-06-29 | 安徽新大陆特种涂料有限责任公司 | Preparation method of anticorrosive antistatic machine tool coating |
| CN114639555A (en) * | 2022-02-24 | 2022-06-17 | 长春工业大学 | Porous thin layer reduced graphene oxide, carbon fiber flexible electrode material and preparation method thereof |
| CN114639555B (en) * | 2022-02-24 | 2023-12-08 | 长春工业大学 | Porous thin-layer reduced graphene oxide, carbon fiber flexible electrode material and preparation method thereof |
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Application publication date: 20140416 |