CN103833019A - Graphene and preparation method thereof - Google Patents
Graphene and preparation method thereof Download PDFInfo
- Publication number
- CN103833019A CN103833019A CN201210484413.2A CN201210484413A CN103833019A CN 103833019 A CN103833019 A CN 103833019A CN 201210484413 A CN201210484413 A CN 201210484413A CN 103833019 A CN103833019 A CN 103833019A
- Authority
- CN
- China
- Prior art keywords
- graphene
- preparation
- sample
- surface area
- specific surface
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the field of electrochemistry, and discloses graphene and a preparation method thereof. The preparation method of the composite material comprises the following steps: putting graphite oxide in a reactor in an inert atmosphere; performing addition treatment to the graphite oxide; adding vapor into the reactor to perform activation treatment to obtain a graphene sample; performing vacuum drying treatment to the graphene sample to obtain the graphene. According to the graphene preparation method, graphene with high specific surface area can be obtained; the preparation method does not need equipment with strong corrosion resistance, so that the investment cost for equipment can be reduced, and the service life of the equipment can be prolonged; the adopted vapor does not hurt environment or human beings, and can be directly emitted to the air, so that the tail gas treatment cost can be reduced.
Description
Technical field
The present invention relates to Graphene field, relate in particular to a kind of Graphene and preparation method thereof.
Background technology
Graphene is a kind of two-dimentional unimolecular layer material, all formed by carbon atom, to find at present the thinnest material, this makes Graphene have excellent character, as high-specific surface area, high conductivity, the toughness of high mechanical strength and excellence etc., there is the potential of application in a lot of fields, be therefore subject to investigator's extensive concern.The theoretical specific surface area of Graphene can reach 2630m2/g, but the specific surface area of in fact prepared Graphene is well below this numerical value, only has 600m2/g left and right, and this has restricted the application of Graphene greatly.Depend primarily on the number of plies of Graphene and the reunion of Graphene by the specific surface area of the prepared Graphene of the whole bag of tricks, the number of plies of Graphene is less, and specific surface area is higher; The reunion degree of Graphene is lower, and specific surface area is higher.At present, the Graphene that the number of plies is can be realized by some preparation methods, and the method that this problem has never had but Graphene is reunited solves, and this has limited greatly, and Graphene advances and widespread use.
Up to the present, known to the method for preparing Graphene have multiple, as (1) micromechanics stripping method.This method can only produce the very limited graphene film of quantity, can be used as fundamental research; (2) ultrahigh vacuum(HHV) Graphene epitaxial growth method.The structural limitations of the expensive and sequin of this method its application; (3) chemical Vapor deposition process (CVD).This method can meet the requirement that high-quality graphene is prepared in mass-producing, but cost is higher, complex process.(4) solvent stripping method.This method shortcoming is that productive rate is very low, limits its commercial applications; (5) oxidation-reduction method.This method is a kind of common method that the most simply can obtain in a large number Graphene, more conventional method of reducing is chemical reduction (hydrazine hydrate, quadrol, sodium borohydride etc. make reductive agent) and Rapid Thermal reduction, but after the whole bag of tricks reduction, all can there is the process of a reunion in Graphene, cause the specific surface area of Graphene less than normal, be generally less than 900m
2/ g.
Summary of the invention
Based on the problems referred to above, problem to be solved by this invention is to provide the preparation method of the Graphene that a kind of specific surface area is higher.
Technical scheme of the present invention is as follows:
A preparation method for Graphene, comprises the steps:
First, graphite oxide is placed in to the reactor of inert atmosphere;
Subsequently, at 800 ~ 1000 ℃, graphite oxide is carried out to heat treated,
Then, then pass into water vapour in reactor, carry out activation treatment 30 ~ 120min, after activation treatment is complete, drop to room temperature, obtain Graphene sample;
Finally, Graphene sample is carried out to drying treatment, obtain Graphene.
Preferably, described Graphene, wherein, when described heat treated, Heating temperature is to be warming up to 800 ~ 1000 ℃ with the heat-up rate of 5 ~ 15 ℃/min.
Preferably, the preparation method of described Graphene, wherein, described drying treatment is to carry out in vacuum drying oven, and drying temperature is 80 ~ 120 ℃, be 8 ~ 12h time of drying.
Preferably, the preparation method of described Graphene, wherein, described inert atmosphere comprises the inert atmosphere that nitrogen, argon gas and nitrogen and argon gas gas mixture form.
The present invention also provides a kind of Graphene, and this Graphene adopts above-mentioned preparation method to make.
The preparation method of Graphene provided by the invention, the method adopts water vapour to activate and can realize high-specific surface area equally raw material, and the specific surface area of the Graphene obtaining is 1000 ~ 2000m
2/ g, Graphene the specific surface area (~ 900m preparing higher than ordinary method
2/ g), can be used for the aspect such as electrode materials and cathode of lithium battery of ultracapacitor.This preparation method does not need to adopt the equipment of strong corrosion resistant, has reduced the input cost of equipment, has increased the work-ing life of equipment simultaneously; The water vapour adopting is all safe from harm to environment and people, can directly be discharged in atmosphere, has reduced vent gas treatment cost.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of Graphene of the present invention;
Fig. 2 is the SEM figure of the Graphene that makes of embodiment 1.
Embodiment
The preparation method of Graphene provided by the invention, as shown in Figure 1, its processing step is as follows:
S1, graphite oxide is put into reactor, in the preferred retort furnace of the present invention, then in retort furnace, pass into 30 ~ 60 minutes rare gas elementes, as nitrogen, argon gas or nitrogen and argon gas gas mixture, to discharge the air in retort furnace, make formation inert atmosphere in retort furnace;
S2, be warming up to 800 ~ 1000 ℃ with the heat-up rate of 5 ~ 15 ℃/min, graphite oxide is added to processing;
S3, stop passing into rare gas element, then in retort furnace, pass into water vapour, carry out activation treatment 30 ~ 120min, after activation treatment is complete, stops passing into water vapour, more then pass into rare gas element, and drop to room temperature in the protection of rare gas element, obtain Graphene sample;
S4, wherein, puts into 80 ~ 120 ℃ of vacuum drying oven inherences vacuum drying treatment 8 ~ 12 hours by Graphene sample, obtains Graphene.
The preparation method of Graphene provided by the invention, the method adopts water vapour to activate and can realize high-specific surface area equally raw material, and the specific surface area of the Graphene obtaining is 1000 ~ 2000m
2/ g, Graphene the specific surface area (~ 900m preparing higher than ordinary method
2/ g), can be used for the aspect such as electrode materials and cathode of lithium battery of ultracapacitor.This preparation method does not need to adopt the equipment of strong corrosion resistant, has reduced the input cost of equipment, has increased the work-ing life of equipment simultaneously; The water vapour adopting is all safe from harm to environment and people, can directly be discharged in atmosphere, has reduced vent gas treatment cost.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
40g raw material is added in retort furnace, first in retort furnace, pass into nitrogen to drive wherein air, after 30 minutes, start heating, be warming up to 800 ℃ with 5 ℃/min speed; Then passing into water vapour activates; at the temperature of 800 ℃, activate after 120min; stop heating; air-flow is switched to nitrogen; drop to room temperature in nitrogen protection; obtain Graphene sample, then sample is put into the inherent 80 ℃ of vacuum-dryings of vacuum drying oven 12 hours, obtain the Graphene of high-specific surface area.
Fig. 2 is the SEM figure of the Graphene that makes of embodiment 1; As shown in Figure 2, Graphene has been stripped from out completely, and has formed higher specific surface area through carbon dioxide activation.
Embodiment 2
40g raw material is added in retort furnace, first in retort furnace, pass into argon gas to drive wherein air, after 60 minutes, start heating, be warming up to 1000 ℃ with 15 ℃/min speed; Then passing into water vapour activates; at the temperature of 1000 ℃, activate after 30min; stop heating; air-flow is switched to argon gas; drop to room temperature in nitrogen protection; obtain Graphene sample, then sample is put into the inherent 120 ℃ of vacuum-dryings of vacuum drying oven 8 hours, obtain the Graphene of high-specific surface area.
Embodiment 3
40g raw material is added in retort furnace, first, to passing into nitrogen and argon gas mixed gas in retort furnace to drive wherein air, after 35 minutes, start heating, be warming up to 850 ℃ with 6 ℃/min speed; Then passing into water vapour activates; at the temperature of 850 ℃, activate after 100min; stop heating; air-flow is switched to nitrogen and argon gas mixed gas; obtain Graphene sample; in nitrogen and the mixed gas protected room temperature that drops to of argon gas, then sample is put into the inherent 85 ℃ of vacuum-dryings of vacuum drying oven 11 hours, obtain the Graphene of high-specific surface area.
Embodiment 4
40g raw material is added in retort furnace, first in retort furnace, pass into nitrogen to drive wherein air, after 40 minutes, start heating, be warming up to 870 ℃ with 8 ℃/min speed; Then passing into water vapour activates; at the temperature of 870 ℃, activate after 90min; stop heating; air-flow is switched to nitrogen; drop to room temperature in nitrogen protection; obtain Graphene sample, then sample is put into the inherent 90 ℃ of vacuum-dryings of vacuum drying oven 11 hours, obtain the Graphene of high-specific surface area.
Embodiment 5
40g raw material is added in retort furnace, first in retort furnace, pass into nitrogen to drive wherein air, after 45 minutes, start heating, be warming up to 900 ℃ with 10 ℃/min speed; Then passing into water vapour activates; at the temperature of 900 ℃, activate after 75min; stop heating; air-flow is switched to nitrogen; drop to room temperature in nitrogen protection; obtain Graphene sample, then sample is put into the inherent 100 ℃ of vacuum-dryings of vacuum drying oven 10 hours, obtain the Graphene of high-specific surface area.
Embodiment 6
40g raw material is added in retort furnace, first in retort furnace, pass into nitrogen to drive wherein air, after 50 minutes, start heating, be warming up to 950 ℃ with 12 ℃/min speed; Then passing into water vapour activates; at the temperature of 950 ℃, activate after 60min; stop heating; air-flow is switched to nitrogen; drop to room temperature in nitrogen protection; obtain Graphene sample, then sample is put into the inherent 110 ℃ of vacuum-dryings of vacuum drying oven 9 hours, obtain the Graphene of high-specific surface area.
Embodiment 7
40g raw material is added in retort furnace, first in retort furnace, pass into nitrogen to drive wherein air, after 55 minutes, start heating, be warming up to 980 ℃ with 14 ℃/min speed; Then passing into water vapour activates; at the temperature of 980 ℃, activate after 40min; stop heating; air-flow is switched to nitrogen; drop to room temperature in nitrogen protection; obtain Graphene sample, then sample is put into the inherent 115 ℃ of vacuum-dryings of vacuum drying oven 8 hours, obtain the Graphene of high-specific surface area.
The grapheme material of embodiment 1 ~ 7 preparation is tested to the specific surface area obtaining by BET as shown in table 1:
Table 1
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| The specific surface area m of Graphene 2/g | 1050 | 2082 | 1125 | 1235 | 1476 | 1685 | 1867 |
Graphene specific surface area prepared by conventional thermal reduction method is ~ 900m
2/ g, the present invention obtains Graphene specific surface area and has substantially exceeded ordinary method.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (5)
1. a preparation method for Graphene, is characterized in that, comprises the steps:
First, graphite oxide is placed in to the reactor of inert atmosphere:
Subsequently, at 800 ~ 1000 ℃, graphite oxide is carried out to heat treated,
Then, then pass into water vapour in reactor, carry out activation treatment 30 ~ 120min, after activation treatment is complete, drop to room temperature, obtain Graphene sample:
Finally, Graphene sample is carried out to drying treatment, obtain Graphene.
2. the preparation method of Graphene according to claim 1, is characterized in that, when described heat treated, Heating temperature is to be warming up to 800 ~ 1000 ℃ with the heat-up rate of 5 ~ 15 ℃/min.
3. the preparation method of Graphene according to claim 1, is characterized in that, described drying treatment is to carry out in vacuum drying oven, and drying temperature is 80 ~ 120 ℃, and be 8 ~ 12h time of drying.
4. according to the preparation method of the Graphene described in claim 1,2 or 3, it is characterized in that, described inert atmosphere comprises the inert atmosphere that nitrogen, argon gas and nitrogen and argon gas gas mixture form.
5. a Graphene, is characterized in that, this Graphene adopts the arbitrary described preparation method of claim 1 ~ 4 to make.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210484413.2A CN103833019A (en) | 2012-11-23 | 2012-11-23 | Graphene and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210484413.2A CN103833019A (en) | 2012-11-23 | 2012-11-23 | Graphene and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103833019A true CN103833019A (en) | 2014-06-04 |
Family
ID=50796967
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210484413.2A Pending CN103833019A (en) | 2012-11-23 | 2012-11-23 | Graphene and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103833019A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104215727A (en) * | 2014-09-25 | 2014-12-17 | 深圳粤网节能技术服务有限公司 | Graphene material based disperse and quick solid-phase extraction method |
| WO2016045030A1 (en) * | 2014-09-25 | 2016-03-31 | 深圳粤网节能技术服务有限公司 | Graphene material-based dispersive solid phase extraction method |
| WO2016045032A1 (en) * | 2014-09-25 | 2016-03-31 | 深圳粤网节能技术服务有限公司 | Solid phase extraction column, preparation method therefor, and chemical sample pre-processing method based on solid phase extraction column |
| WO2023078159A1 (en) * | 2021-11-08 | 2023-05-11 | 湖南中科星城石墨有限公司 | Artificial graphite negative electrode material, preparation method, and use |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070140A (en) * | 2011-02-28 | 2011-05-25 | 无锡第六元素高科技发展有限公司 | Method for preparing high-specific surface area graphene material by utilizing strong base chemical treatment |
| CN102543483A (en) * | 2012-01-17 | 2012-07-04 | 电子科技大学 | Preparation method of graphene material of supercapacitor |
| CN102627273A (en) * | 2012-04-19 | 2012-08-08 | 常州第六元素材料科技股份有限公司 | Purifying process for graphene material of energy storing device |
-
2012
- 2012-11-23 CN CN201210484413.2A patent/CN103833019A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070140A (en) * | 2011-02-28 | 2011-05-25 | 无锡第六元素高科技发展有限公司 | Method for preparing high-specific surface area graphene material by utilizing strong base chemical treatment |
| CN102543483A (en) * | 2012-01-17 | 2012-07-04 | 电子科技大学 | Preparation method of graphene material of supercapacitor |
| CN102627273A (en) * | 2012-04-19 | 2012-08-08 | 常州第六元素材料科技股份有限公司 | Purifying process for graphene material of energy storing device |
Non-Patent Citations (1)
| Title |
|---|
| TAE HEE HAN ET AL: "Steam Etched Porous Graphene Oxide Network for Chemical Sensing", 《JACS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104215727A (en) * | 2014-09-25 | 2014-12-17 | 深圳粤网节能技术服务有限公司 | Graphene material based disperse and quick solid-phase extraction method |
| CN104215727B (en) * | 2014-09-25 | 2015-11-25 | 深圳粤网节能技术服务有限公司 | The quick solid phase extraction method of dispersion based on grapheme material |
| WO2016045030A1 (en) * | 2014-09-25 | 2016-03-31 | 深圳粤网节能技术服务有限公司 | Graphene material-based dispersive solid phase extraction method |
| WO2016045032A1 (en) * | 2014-09-25 | 2016-03-31 | 深圳粤网节能技术服务有限公司 | Solid phase extraction column, preparation method therefor, and chemical sample pre-processing method based on solid phase extraction column |
| WO2023078159A1 (en) * | 2021-11-08 | 2023-05-11 | 湖南中科星城石墨有限公司 | Artificial graphite negative electrode material, preparation method, and use |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103833019A (en) | Graphene and preparation method thereof | |
| CN104071786B (en) | A kind of preparation method of greying gac | |
| WO2015196853A1 (en) | Preparation method for lithium iron phosphate | |
| CN103937258A (en) | Conductive silicone rubber with high elastic resilience and preparation method thereof | |
| CN103991860A (en) | Nitrogen-doped graphene and preparation method thereof | |
| CN103949209A (en) | Plant based carbon material and preparation method thereof | |
| CN105752969A (en) | Method for preparing polyatomic self-doped graphene by using natural porous and laminated vegetables | |
| CN105984866B (en) | Surface Modification Method of Graphene | |
| CN104084197A (en) | Ruthenium system ammonia synthesis catalyst using graphitization activated carbon as carrier and preparation method of catalyst | |
| CN107217330A (en) | Composite nano-line of transition metal and graphene and preparation method thereof | |
| CN104030265B (en) | Nitrogen-doped carbon nanometer pipe and preparation method thereof | |
| CN106044744A (en) | Preparation method and application of graphene-lignin-based composite hierarchical pore carbon plate material | |
| CN102464312A (en) | Preparation method of graphene | |
| CN104030263A (en) | Nitrogen-doped carbon nanotube and preparation method thereof | |
| CN103771398A (en) | Boron-doped graphene, and preparation method and application thereof | |
| CN103165866A (en) | Nitrogen doped graphene/metal composite electrode and its preparation method | |
| CN103833015A (en) | Graphene and preparation method thereof | |
| CN102923693A (en) | Surface modification treatment method for graphene | |
| CN103833017A (en) | Boron-doped graphene and preparation method thereof | |
| CN108946727B (en) | Method for preparing activated carbon by using microalgae-alginate complex | |
| CN103991861A (en) | Nitrogen-doped graphene and preparation method thereof | |
| CN104064367A (en) | Nitrogen doped carbon nanotube/ionic liquid composite film and preparation method thereof, and capacitor | |
| CN104030692A (en) | Method for synthesizing ultrahigh temperature ceramic hybridization powder containing graphene oxide and carbon nano tubes in situ | |
| CN104671238B (en) | Method for quickly preparing high-performance graphene | |
| CN104148039A (en) | Method for acquiring activated regenerated paracetamol pharmaceutical waste activated carbon through microwave heating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140604 |