CN103482610A - Graphene preparation method - Google Patents
Graphene preparation method Download PDFInfo
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- CN103482610A CN103482610A CN201210196561.4A CN201210196561A CN103482610A CN 103482610 A CN103482610 A CN 103482610A CN 201210196561 A CN201210196561 A CN 201210196561A CN 103482610 A CN103482610 A CN 103482610A
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Abstract
The invention discloses a graphene preparation method. The method comprises the following steps: mixing graphite with an interhalogen compound to obtain a mixture, sealing, placing the mixture in 100-160DEG C environment, reacting for 48-60h, cooling to obtain a graphite intercalated compound; and heating the graphite intercalated compound to 700-900DEG C under a protection gas, reacting for 0.5-1h, and cooling to obtain graphene. The graphene preparation method allows graphene to be prepared by preparing the graphite intercalated compound through using graphite and the interhalogen compound, heating the graphite intercalated compound to 700-900DEG C, reacting for 0.5-1h and cooling. The layer number of the graphene prepared in the invention is lower than that of traditional graphene prepared through a liquid phase method, and is only 2-3. Additionally, the graphene preparation method has the advantages of high yield, simple used apparatus and technology, convenient operation, cheap raw materials, low cost, and easy realization of the large-scale industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene.
Background technology
Graphene is a kind of two-dimentional unimolecular layer material, has excellent physical properties, as high theoretical specific surface area, excellent physical strength, good snappiness and high specific conductivity etc., is subject to investigator's extensive concern.The method for preparing at present Graphene mainly contains mechanically peel method, epitaxial growth method, oxidation reduction process and chemical Vapor deposition process, utilizes mechanically peel method and epitaxial growth method to prepare the amount of Graphene lower, and in uneven thickness; Oxidation reduction process mainly is divided into heat of oxidation reduction and oxidation chemistry reduction, heat of oxidation reduction method prepares the temperature that Graphene is often had relatively high expectations, energy consuming ratio is larger, and the chemical preparation Graphene often adopts the chemical reagent such as hydrazine, these reagent have certain toxicity, and human body and environment are brought to harm; Use process for preparing graphenes by chemical vapour deposition, production unit is had relatively high expectations.
The environmental protection of Liquid preparation methods Graphene, low for equipment requirements, consuming time short, be a kind of comparatively excellent Graphene method for preparing.
Yet the number of plies of the Graphene that adopts Liquid preparation methods to obtain is higher.
Summary of the invention
Based on this, be necessary to provide a kind of preparation method that can prepare the Graphene of the Graphene that the number of plies is lower.
A kind of preparation method of Graphene, comprise the steps:
Will graphite and interhalogen compounds mix after sealing, then mixture is placed under the environment of 100 ℃～160 ℃ and reacts 48h～60h, obtain graphite intercalation compound after cooling;
Passing under the condition of shielding gas, described graphite intercalation compound is being warming up to 700 ℃～900 ℃ reaction 0.5h～1h, obtaining Graphene after cooling.
In one embodiment, described graphite and described interhalogen compounds mix according to mass ratio 5:3～5.
In one embodiment, described interhalogen compounds is at least one in iodine bromide IBr and iodine chloride.
In one embodiment, described graphite and interhalogen compounds are mixed after being operating as of sealing: after graphite and interhalogen compounds are mixed in the tetrafluoroethylene bottle by described tetrafluoroethylene bottle closure.
In one embodiment, the flow of described shielding gas is 300mL/min～400mL/min.
In one embodiment, described shielding gas is argon gas or nitrogen.
In one embodiment, described described graphite intercalation compound being warming up in the step of 700 ℃～900 ℃, temperature rise rate is 20 ℃/min～30 ℃/min.
In one embodiment, the described step that obtains Graphene after cooling is: be cooled to room temperature under the shielding gas atmosphere, obtain Graphene.
The preparation method of this Graphene prepares graphite intercalation compound by graphite and interhalogen compounds, then graphite intercalation compound is warming up to 700 ℃～900 ℃ reaction 0.5h～1h, makes Graphene after cooling.With respect to the Graphene of traditional employing Liquid preparation methods, the Graphene number of plies made is lower, is only generally 2 layers～3 layers.In addition, preparation method's productive rate of this Graphene is higher, and equipment, the technique of use are simple, convenient operation, and the cheap cost of raw material is low, easily realizes large-scale industrial production.
The accompanying drawing explanation
The preparation method's of the Graphene that Fig. 1 is an embodiment schema;
The number of plies distribution plan of the Graphene that Fig. 2 is embodiment 1 preparation;
The transmission electrode photo of the Graphene that Fig. 3 is embodiment 1 preparation.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.A lot of details have been set forth in the following description so that fully understand the present invention.But the present invention can implement much to be different from alternate manner described here, those skilled in the art can be in the situation that do similar improvement without prejudice to intension of the present invention, so the present invention is not subject to the restriction of following public concrete enforcement.
The preparation method of the Graphene of an embodiment as shown in Figure 1, comprise the steps:
S10, will graphite and interhalogen compounds mix after sealing, then mixture is placed under the environment of 100 ℃～160 ℃ and reacts 48h～60h, obtain graphite intercalation compound after cooling.
Graphite generally selects purity at 99.5% graphite.
Interhalogen compounds can be at least one in iodine bromide IBr and iodine chloride.
Graphite and interhalogen compounds can mix according to mass ratio 5:3～5.
Can adopt the container of tetrafluoroethylene bottle as graphite and interhalogen compounds, after graphite and interhalogen compounds are mixed in the tetrafluoroethylene bottle by the tetrafluoroethylene bottle closure, the tetrafluoroethylene bottle that mixture then will be housed is placed under the environment of 100 ℃～160 ℃ and reacts 48h～60h, obtains graphite intercalation compound after cooling.
The inertia of tetrafluoroethylene is very strong, adopts the tetrafluoroethylene bottle higher as reaction vessel stability.
S20, passing under the condition of shielding gas, the graphite intercalation compound that S10 is obtained is warming up to 700 ℃～900 ℃ reaction 0.5h～1h, obtains Graphene after cooling.
The flow of shielding gas is 300mL/min～400mL/min.
Shielding gas can be argon gas or nitrogen.
Graphite intercalation compound is warming up in the step of 700 ℃～900 ℃, temperature rise rate can be 20 ℃/min～30 ℃/min.
The step that obtains Graphene after cooling is: be cooled to room temperature under the shielding gas atmosphere, obtain Graphene.
The preparation method of this Graphene prepares graphite intercalation compound by graphite and interhalogen compounds, then graphite intercalation compound is warming up to 700 ℃～900 ℃ reaction 0.5h～1h, makes Graphene after cooling.With respect to the Graphene of traditional employing Liquid preparation methods, the Graphene number of plies made is lower, is only generally 2 layers～3 layers.In addition, preparation method's productive rate of this Graphene is higher, and equipment, the technique of use are simple, convenient operation, and the cheap cost of raw material is low, easily realizes large-scale industrial production.
It is below specific embodiment.
Embodiment 1
Graphite, 4g iodine chloride that to take 5g purity be 99.5% add in the tetrafluoroethylene bottle successively, and bottle is sealed, the tetrafluoroethylene bottle is placed under the envrionment temperature of 150 ℃ to reaction 48h, afterwards the temperature of tetrafluoroethylene bottle is down to room temperature, obtains graphite intercalation compound.
The graphite intercalation compound of preparation is placed under argon gas (400mL/min) atmosphere, and with the temperature rise rate of 30 ℃/min, the envrionment temperature of graphite intercalation compound is risen to 900 ℃, keep 0.5h, then in argon gas (400mL/min) atmosphere, drop to room temperature, obtain Graphene.
The thickness of 100 parts of Graphenes that adopt atomic force microscope to make embodiment 1 is tested, and according to thickness, infers and the Graphene number of plies, obtains Fig. 2.
In 100 parts of Graphenes, be individual layer more than 85% as can be known from Fig. 2, can think that thus the prepared Graphene of the present embodiment is single-layer graphene.
The transmission electrode photo that Fig. 3 is the prepared Graphene of embodiment 1, the number of plies of Graphene is less as can be seen from the figure.
Embodiment 2
Graphite, 6g iodine bromide IBr that to take 10g purity be 99.5% add in the tetrafluoroethylene bottle successively, and bottle is sealed, the tetrafluoroethylene bottle is placed under the envrionment temperature of 100 ℃ to reaction 48h, afterwards the temperature of tetrafluoroethylene bottle is down to room temperature, obtains graphite intercalation compound.
The graphite intercalation compound of preparation is placed under nitrogen (300mL/min) atmosphere, and with the temperature rise rate of 25 ℃/min, the envrionment temperature of graphite intercalation compound is risen to 800 ℃, keep 1h, then in argon gas (300mL/min) atmosphere, drop to room temperature, obtain Graphene.
Graphite, 50g iodine chloride that to take 50g purity be 99.5% add in the tetrafluoroethylene bottle successively, and bottle is sealed, the tetrafluoroethylene bottle is placed under the envrionment temperature of 160 ℃ to reaction 60h, afterwards the temperature of tetrafluoroethylene bottle is down to room temperature, obtains graphite intercalation compound.
The graphite intercalation compound of preparation is placed under nitrogen (300mL/min) atmosphere, and with the temperature rise rate of 20 ℃/min, the envrionment temperature of graphite intercalation compound is risen to 700 ℃, keep 1h, then in argon gas (300mL/min) atmosphere, drop to room temperature, obtain Graphene.
Embodiment 4
Graphite, 3g iodine chloride, 3g iodine bromide IBr that to take 10g purity be 99.5% add in the tetrafluoroethylene bottle successively, and bottle is sealed, the tetrafluoroethylene bottle is placed under the envrionment temperature of 100 ℃, reaction 60h, afterwards the temperature of tetrafluoroethylene bottle is down to room temperature, open the tetrafluoroethylene bottle, obtain graphite intercalation compound.
The graphite intercalation compound of preparation is placed under argon gas (400mL/min) atmosphere, and with the temperature rise rate of 20 ℃/min, the envrionment temperature of graphite intercalation compound is risen to 900 ℃, keep 0.5h, then in argon gas (400mL/min) atmosphere, drop to room temperature, obtain Graphene.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. the preparation method of a Graphene, is characterized in that, comprises the steps:
Will graphite and interhalogen compounds mix after sealing, then mixture is placed under the environment of 100 ℃～160 ℃ and reacts 48h～60h, obtain graphite intercalation compound after cooling;
Passing under the condition of shielding gas, described graphite intercalation compound is being warming up to 700 ℃～900 ℃ reaction 0.5h～1h, obtaining Graphene after cooling.
2. the preparation method of Graphene according to claim 1, is characterized in that, described graphite and described interhalogen compounds mix according to mass ratio 5:3～5.
3. the preparation method of Graphene according to claim 1, is characterized in that, described interhalogen compounds is at least one in iodine bromide IBr and iodine chloride.
4. the preparation method of Graphene according to claim 1, is characterized in that, described graphite and interhalogen compounds are mixed after being operating as of sealing: after graphite and interhalogen compounds are mixed in the tetrafluoroethylene bottle by described tetrafluoroethylene bottle closure.
5. the preparation method of Graphene according to claim 1, is characterized in that, the flow of described shielding gas is 300mL/min～400mL/min.
6. the preparation method of Graphene according to claim 1, is characterized in that, described shielding gas is argon gas or nitrogen.
7. the preparation method of Graphene according to claim 1, is characterized in that, described described graphite intercalation compound being warming up in the step of 700 ℃～900 ℃, and temperature rise rate is 20 ℃/min～30 ℃/min.
8. the preparation method of Graphene according to claim 1, is characterized in that, the described step that obtains Graphene after cooling is: be cooled to room temperature under the shielding gas atmosphere, obtain Graphene.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600781A (en) * | 2016-03-02 | 2016-05-25 | 合肥国轩高科动力能源有限公司 | Method for preparing single-layer graphene through CO2 intercalation assisted by ball milling |
| CN108314025A (en) * | 2018-04-24 | 2018-07-24 | 盐城师范学院 | A kind of preparation method of bilayer graphene intercalation compound |
| CN108467031A (en) * | 2018-04-24 | 2018-08-31 | 盐城师范学院 | A kind of preparation method of N-shaped and three layer graphene intercalation compound of p-type |
| CN108516540A (en) * | 2018-04-24 | 2018-09-11 | 盐城师范学院 | A kind of preparation method of dispersible graphene intercalation compound |
| CN109012496A (en) * | 2018-09-29 | 2018-12-18 | 盐城师范学院 | A kind of method that shock wave method prepares diamond thin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431999A (en) * | 2011-09-22 | 2012-05-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
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- 2012-06-14 CN CN201210196561.4A patent/CN103482610A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431999A (en) * | 2011-09-22 | 2012-05-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105600781A (en) * | 2016-03-02 | 2016-05-25 | 合肥国轩高科动力能源有限公司 | Method for preparing single-layer graphene through CO2 intercalation assisted by ball milling |
| CN108314025A (en) * | 2018-04-24 | 2018-07-24 | 盐城师范学院 | A kind of preparation method of bilayer graphene intercalation compound |
| CN108467031A (en) * | 2018-04-24 | 2018-08-31 | 盐城师范学院 | A kind of preparation method of N-shaped and three layer graphene intercalation compound of p-type |
| CN108516540A (en) * | 2018-04-24 | 2018-09-11 | 盐城师范学院 | A kind of preparation method of dispersible graphene intercalation compound |
| CN108516540B (en) * | 2018-04-24 | 2020-12-08 | 盐城师范学院 | Preparation method of dispersible graphene intercalation compound |
| CN109012496A (en) * | 2018-09-29 | 2018-12-18 | 盐城师范学院 | A kind of method that shock wave method prepares diamond thin |
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Application publication date: 20140101 |