CN104085886B - Graphene and preparation method thereof - Google Patents
Graphene and preparation method thereof Download PDFInfo
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- CN104085886B CN104085886B CN201410363993.9A CN201410363993A CN104085886B CN 104085886 B CN104085886 B CN 104085886B CN 201410363993 A CN201410363993 A CN 201410363993A CN 104085886 B CN104085886 B CN 104085886B
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Abstract
The invention discloses a kind of Graphene and preparation method thereof, comprising: 1) graphite composite powder is mixed with aluminum chloride, under protection of inert gas, heat 5 ~ 95 hours under 200 ~ 300 DEG C of conditions, be then cooled to 20 ~ 30 DEG C; 2) continue to add low-carbon (LC) nitroparaffins, stir 3 ~ 70 hours under 20 ~ 30 DEG C of conditions, obtain intercalation mixture; 3) adopt intercalation mixture described in carry out microwave radiation heating, obtain expanded graphite, then this expanded graphite is placed in water strong stirring, be i.e. obtained graphene suspension.Preparation method's tool provided by the invention has the following advantages: (1) operating process simply, is easily controlled, and aftertreatment is simple, and the quality of Graphene is high; (2) little to the hazardness of environment and people; (3) proper scaleization preparation; (4) be convenient to store and transport.
Description
Technical field
The present invention relates to technical field of nano material, particularly relate to a kind of Graphene and preparation method thereof.
Background technology
Graphene is the full carbon material of a kind of widely used two dimension, but this material of a large amount of preparation still exists the high problem of cost.Most report is that preparation after graphite oxidation is contained the Graphene of a large amount of defect and functional group, minority reports that useful electrochemical process or graphite intercalation method obtain Graphene, wherein preparing with graft process the intercalated material that Graphene uses is metallic lithium, butyllithium or iron(ic) chloride, the above two materials are not only expensive, and chance water is inflammable easily sudden and violent, then a kind of material then needs higher temperature when intercalation, and iron(ic) chloride is to plant and instrument seriously corroded, interact with the carbon atom in graphite again very strong, therefore, not only preparation process is very complicated, and aftertreatment is also very loaded down with trivial details and difficult, be difficult to simply peel off graphite and obtain the Graphene of high-quality.
Summary of the invention
In view of this, the object of the invention is to the preparation method proposing a kind of Graphene, obviously to simplify the preparation process of Graphene, improve the quality of Graphene simultaneously.
Based on above-mentioned purpose, the preparation method of Graphene provided by the invention comprises the following steps:
1) graphite composite powder is mixed with aluminum chloride, under protection of inert gas, heat 5 ~ 95 hours under 200 ~ 300 DEG C of conditions, be then cooled to 20 ~ 30 DEG C;
2) continue to add low-carbon (LC) nitroparaffins, stir 3 ~ 70 hours under 20 ~ 30 DEG C of conditions, obtain intercalation mixture;
3) adopt intercalation mixture described in carry out microwave radiation heating, obtain expanded graphite powder, then this expanded graphite is placed in water strong stirring, be i.e. obtained graphene suspension.
Alternatively, the mass ratio of described graphite composite powder and aluminum chloride is 1:3 ~ 10.
Preferably, the quality of described graphite composite powder is 2 ~ 10 grams per milliliters with the ratio of the volume of low-carbon (LC) nitroparaffins.
Preferably, described low-carbon (LC) nitroparaffins are selected from least one in Nitromethane 99Min., nitroethane and nitropropane.
Alternatively, described step 2) in stirring velocity be 500 ~ 2000 revs/min, described step 3) in stirring velocity be 6000 ~ 15000 revs/min.
Preferably, described step 3) after also comprise: obtain graphene powder by after centrifugal for described graphene suspension, vacuum-drying.
Alternatively, heated mixt to 200 ~ 350 DEG C under microwave radiation, and keep 2 ~ 10 minutes.
Preferably, described microwave radiation is carried out in atmosphere, and the wavelength of described microwave is 100 ~ 200mm, and frequency is 2200 ~ 2800MHz.
The present invention also provides a kind of Graphene, and described Graphene obtains according to the preparation method of above-mentioned Graphene.
As can be seen from above, graphene preparation method provided by the invention is by mixing graphite with Aluminum chloride anhydrous, and heat in rare gas element, aluminum chloride molecule just can be inserted into graphite layers and obtain aluminum chloride intercalation thing under lower temperature of reaction; Again by aluminum chloride molecule between small organic molecule part substituted layer, make organic substance decomposing under heating, and then allow graphite expansion peel off, thus obtained Graphene.Or directly microwave heating aluminum chloride intercalation thing, obtains expanded graphite because aluminum chloride gasifies rapidly, thus obtained Graphene.Because the aluminum chloride molecule being in interlayer is unstable, carbon atom in aluminum chloride and graphite interacts more weak, easy and low-carbon (LC) nitroparaffins generating portion exchanges, and then make low-carbon (LC) nitroparaffins be embedded in graphite layers, make the low-carbon (LC) nitroparaffins of interlayer decompose in a heated condition, impel graphite expansion and peel off the rear Graphene that just can obtain high-quality.Therefore, preparation method's tool provided by the invention has the following advantages: (1) operating process simply, is easily controlled, and aftertreatment is simple, and the quality of Graphene is high; (2) little to the hazardness of environment and people; (3) proper scaleization preparation; (4) be convenient to store and transport.
Accompanying drawing illustrates:
Fig. 1 is the scanning electron microscope diagram of raw materials used graphite composite powder under 100 multiples in the embodiment of the present invention;
Fig. 2 is the scanning electron microscope diagram of raw materials used graphite composite powder under 500 multiples in the embodiment of the present invention;
Fig. 3 is the scanning electron microscope diagram of raw materials used graphite composite powder under 1000 multiples in the embodiment of the present invention
Fig. 4 is the scanning electron microscope diagram of Graphene under 500 multiples that the embodiment of the present invention obtains;
Fig. 5 is the scanning electron microscope diagram of Graphene under 1000 multiples that the embodiment of the present invention obtains;
Fig. 6 is the scanning electron microscope diagram of Graphene under 100000 multiples that the embodiment of the present invention obtains;
Fig. 7 is the transmission electron microscope figure of the Graphene that the embodiment of the present invention obtains;
Fig. 8 is the X ray diffracting spectrum of embodiment of the present invention raw material sheet graphite composite powder and obtained Graphene.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
Embodiment 1
First, under high pure nitrogen protection, by 2 grams of graphite composite powders and 16 grams of anhydrous AlCl
3join in reactor and mix, heat 63 hours at 250 DEG C; After naturally cooling to 25 DEG C, continue in reactor, add 10 milliliters of Nitromethane 99Min.s, stir 29 hours with the speed of 1500 revs/min at 25 DEG C after, from reactor, take out intercalation mixture; Then about heating intercalation mixture to 260 DEG C in atmosphere under microwave radiation, and keep 4 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water and stirs with the speed of 8500 revs/min, be i.e. the graphene suspension of obtained favorable dispersity, obtain graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.Preferably, described aluminum chloride is Aluminum chloride anhydrous.Wherein, the wavelength of described microwave is 150mm, and frequency is 2200MHz.It should be noted that, also directly intercalation mixture can be put into microwave oven, in atmosphere, under normal pressure microwave heating obtain expanded graphite.
Embodiment 2
First, under high-purity argon gas protection, by 2 grams of graphite composite powders and 17 grams of anhydrous AlCl
3join in reactor and mix, heat 26 hours at 290 DEG C; After naturally cooling to 27 DEG C, continue in reactor, add 15 milliliters of Nitromethane 99Min.s, stir 29 hours with the speed of 650 revs/min at 26 DEG C after, from reactor, take out intercalation mixture; Then about heating intercalation mixture to 220 DEG C in atmosphere under microwave radiation, and keep 5 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water and stirs with the speed of 10000 revs/min, be i.e. the graphene suspension of obtained favorable dispersity, obtain graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.Wherein, the wavelength of described microwave is 125mm, and frequency is 2600MHz.
Embodiment 3
First, under high pure nitrogen protection, by 3 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, heat 52 hours at 260 DEG C; After naturally cooling to 23 DEG C, continue in reactor, add 16 milliliters of Nitromethane 99Min.s, stir 62 hours with the speed of 550 revs/min at 27 DEG C after, from reactor, take out intercalation mixture; Then about heating intercalation mixture to 250 DEG C in atmosphere under microwave radiation, and keep 4.5 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water and stirs with the speed of 10650 revs/min, be i.e. the graphene suspension of obtained favorable dispersity, obtain graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.Wherein, the wavelength of described microwave is 130mm, and frequency is 2400MHz.It should be noted that, also directly intercalation mixture can be put into microwave oven, in atmosphere, under normal pressure microwave heating obtain expanded graphite.
Embodiment 4
First, under high pure nitrogen protection, by 5 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, heat 17 hours at 300 DEG C; After naturally cooling to 28 DEG C, continue in reactor, add 16 milliliters of nitroethanes, stir 55 hours with the speed of 820 revs/min at 27 DEG C after, from reactor, take out intercalation mixture; Then about heating intercalation mixture to 300 DEG C in atmosphere under microwave radiation, and keep 4 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water and stirs with the speed of 12360 revs/min, be i.e. the graphene suspension of obtained favorable dispersity, obtain graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.
Embodiment 5
First, under high pure nitrogen protection, by 2.5 grams of graphite composite powders and 18 grams of anhydrous AlCl
3join in reactor and mix, heat 24 hours at 265 DEG C; Take out after naturally cooling to 25.2 DEG C, in atmosphere under microwave radiation about heated mixt to 230 DEG C, and keep 4 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water with 11000 revs/min of stirrings, i.e. the graphene suspension of obtained favorable dispersity, obtains graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.Wherein, the wavelength of described microwave is 110 ~ 160mm, and frequency is 2300 ~ 2600MHz.
Embodiment 6
First, under high pure nitrogen protection, by 2.5 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, heat 25 hours at 290 DEG C; After naturally cooling to 25.2 DEG C, continue in reactor, add 16 milliliters of nitroethanes, stir 72 hours with the speed of 1580 revs/min at 27 DEG C after, from reactor, take out intercalation mixture; Then about heating intercalation mixture to 250 DEG C in atmosphere under microwave radiation, and keep 4 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water and stirs with the speed of 9250 revs/min, be i.e. the graphene suspension of obtained favorable dispersity, obtain graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.Wherein, the wavelength of described microwave is 122mm, and frequency is 2250MHz.It should be noted that, also directly intercalation mixture can be put into microwave oven, in atmosphere, under normal pressure microwave heating obtain expanded graphite.
Embodiment 7
First, under high pure nitrogen protection, by 3 grams of graphite composite powders and 28 grams of anhydrous AlCl
3join in reactor and mix, heat 36 hours at 283 DEG C; After naturally cooling to 26.2 DEG C, continue in reactor, add 13 milliliters of nitropropanes, stir 70 hours with 1260 revs/min at 27 DEG C after, from reactor, take out intercalation mixture; Then about heating intercalation mixture to 260 DEG C in atmosphere under microwave radiation, and keep 4.8 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water and stirs with the speed of 14400 revs/min, be i.e. the graphene suspension of obtained favorable dispersity, obtain graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.Wherein, the wavelength of described microwave is 160mm, and frequency is 2650MHz.It should be noted that, also directly intercalation mixture can be put into microwave oven, in atmosphere, under normal pressure microwave heating obtain expanded graphite.
Embodiment 8
First, under high-purity argon gas protection, by 4 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, heat 95 hours at 200 DEG C; After naturally cooling to 25 DEG C, continue in reactor, add 30 milliliters of nitropropanes, stir 50 hours with the speed of 520 revs/min at 26 DEG C after, from reactor, take out intercalation mixture; Then about heating intercalation mixture to 255 DEG C in atmosphere under microwave radiation, and keep 4.8 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water and stirs with the speed of 7700 revs/min, be i.e. the graphene suspension of obtained favorable dispersity, obtain graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.Wherein, the wavelength of described microwave is 135mm, and frequency is 2440MHz.
Embodiment 9
First, under high pure nitrogen protection, by 3 grams of graphite composite powders and 25 grams of anhydrous AlCl
3join in reactor and mix, heat 63 hours at 250 DEG C; Take out after naturally cooling to 25 DEG C, in atmosphere under microwave radiation about heated mixt to 260 DEG C, and keep 5 minutes, obtain expanded graphite; Finally, the expanded graphite after microwave heating is placed in water and stirs with the speed of 12000 revs/min, be i.e. obtained dispersed graphene suspension preferably, obtain graphene powder by after centrifugal for Graphene suspension liquid, vacuum-drying.Wherein, the wavelength of described microwave is 120 ~ 150mm, and frequency is 2400 ~ 2560MHz.
See Fig. 1 ~ 3, be respectively the scanning electron microscope diagram of raw materials used graphite composite powder under 100 multiples, 500 multiples and 1000 multiples in the embodiment of the present invention; See Fig. 4 ~ 7, be the scanning electron microscope diagram of the Graphene that obtains of the embodiment of the present invention under 500 multiples, 1000 multiples and 100000 multiples and transmission electron microscope figure respectively.
As can be seen from the figure, raw graphite has sheet-like morphology, and the phosphorus flake graphite of size mainly between 0.2 ~ 0.4mm, thickness is also very thick.The Graphene prepared by method provided by the invention then thickness is very thin, has obvious fold to exist.
See Fig. 8, it is the X ray diffracting spectrum of embodiment of the present invention raw graphite powder and obtained Graphene; As can be seen from the figure, the X-ray diffraction peak intensity of raw graphite powder is strong especially, is far better than the intensity at the X-ray diffraction peak of obtained Graphene, and this is because Graphene has the cause of individual layer or several Rotating fields.
As mentioned above, graphene preparation method provided by the invention is by mixing graphite with Aluminum chloride anhydrous, and heat in rare gas element, aluminum chloride molecule just can be inserted into graphite layers and obtain aluminum chloride intercalation thing under lower temperature of reaction; Again by aluminum chloride molecule between small organic molecule part substituted layer, make organic substance decomposing under heating, and then allow graphite expansion peel off, thus obtained Graphene.Or directly microwave heating aluminum chloride intercalation thing, obtains expanded graphite because aluminum chloride gasifies rapidly, thus obtained Graphene.Because the aluminum chloride molecule being in interlayer is unstable, carbon atom in aluminum chloride and graphite interacts more weak, easy and low-carbon (LC) nitroparaffins generating portion exchanges, and then make low-carbon (LC) nitroparaffins be embedded in graphite layers, make the low-carbon (LC) nitroparaffins of interlayer decompose in a heated condition, impel graphite expansion and peel off the rear Graphene that just can obtain high-quality.Therefore, preparation method's tool provided by the invention has the following advantages: (1) operating process simply, is easily controlled, and aftertreatment is simple, and the quality of Graphene is high; (2) little to the hazardness of environment and people; (3) proper scaleization preparation; (4) be convenient to store and transport.
Those of ordinary skill in the field are to be understood that: the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a preparation method for Graphene, is characterized in that, comprises the following steps:
1) graphite composite powder is mixed with aluminum chloride, under protection of inert gas, heat 5 ~ 95 hours under 200 ~ 300 DEG C of conditions, be then cooled to 20 ~ 30 DEG C;
2) continue to add low-carbon (LC) nitroparaffins, stir 3 ~ 70 hours under 20 ~ 30 DEG C of conditions, obtain intercalation mixture;
3) adopt intercalation mixture described in carry out microwave radiation heating, obtain expanded graphite, then this expanded graphite is placed in water strong stirring, be i.e. obtained graphene suspension.
2. the preparation method of Graphene according to claim 1, is characterized in that, the mass ratio of described graphite composite powder and aluminum chloride is 1:3 ~ 10.
3. the preparation method of Graphene according to claim 1, is characterized in that, the quality of described graphite composite powder is 2 ~ 10 grams per milliliters with the ratio of the volume of low-carbon (LC) nitroparaffins.
4. the preparation method of Graphene according to claim 3, is characterized in that, described low-carbon (LC) nitroparaffins are selected from least one in Nitromethane 99Min., nitroethane and nitropropane.
5. the preparation method of Graphene according to claim 1, is characterized in that, described step 2) in stirring velocity be 500 ~ 2000 revs/min, described step 3) in stirring velocity be 6000 ~ 15000 revs/min.
6. the preparation method of Graphene according to claim 1, is characterized in that, described step 3) after also comprise: obtain graphene powder by after centrifugal for described graphene suspension, vacuum-drying.
7. the preparation method of Graphene according to claim 1, is characterized in that, heated mixt to 200 ~ 350 DEG C under microwave radiation, and keeps 2 ~ 10 minutes.
8. the preparation method of Graphene according to claim 1, is characterized in that, described microwave radiation is carried out in atmosphere, and the wavelength of described microwave is 100 ~ 200mm, and frequency is 2200 ~ 2800MHz.
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| CN104477886B (en) * | 2014-11-20 | 2016-09-28 | 中山大学 | A kind of accordion Graphene and controllable method for preparing thereof |
| CN104556010A (en) * | 2014-12-31 | 2015-04-29 | 江苏江大环保科技开发有限公司 | Process for industrially producing graphene by microwaves |
| CN104817074A (en) * | 2015-04-20 | 2015-08-05 | 德阳烯碳科技有限公司 | Process for preparing graphite intercalation compound |
| CN105293482A (en) * | 2015-12-01 | 2016-02-03 | 张扬威 | Solvothermal stripping preparation method of graphene |
| CN106672958A (en) * | 2017-01-18 | 2017-05-17 | 丽水市知科科技有限公司 | Preparation method of graphene oxide |
| CN106744888A (en) * | 2017-01-18 | 2017-05-31 | 丽水市知科科技有限公司 | A kind of preparation method of Graphene |
| CN108622886A (en) * | 2017-03-17 | 2018-10-09 | 国家纳米科学中心 | A kind of liquid nitrogen auxiliary prepares the method for high-quality graphene and high-quality graphene obtained |
| CN113493200A (en) * | 2020-10-17 | 2021-10-12 | 苏州北美国际高级中学 | Preparation method of graphene oxide |
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| CN102583332A (en) * | 2012-01-17 | 2012-07-18 | 北京航空航天大学 | Technology and method for preparing solution used for preparing graphene in liquid phase |
| CN103130213A (en) * | 2011-11-29 | 2013-06-05 | 施乐公司 | Graphene nano-sheets and methods for making the same |
| CN103562130A (en) * | 2012-03-09 | 2014-02-05 | 株式会社大有新素材 | Method for producing planar carbon nanoparticles, and method for producing aluminum/carbon composite material using same |
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| CN103130213A (en) * | 2011-11-29 | 2013-06-05 | 施乐公司 | Graphene nano-sheets and methods for making the same |
| CN102583332A (en) * | 2012-01-17 | 2012-07-18 | 北京航空航天大学 | Technology and method for preparing solution used for preparing graphene in liquid phase |
| CN103562130A (en) * | 2012-03-09 | 2014-02-05 | 株式会社大有新素材 | Method for producing planar carbon nanoparticles, and method for producing aluminum/carbon composite material using same |
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