CN105692602A - Method for simply and rapidly preparing thin graphene - Google Patents
Method for simply and rapidly preparing thin graphene Download PDFInfo
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- CN105692602A CN105692602A CN201610129739.1A CN201610129739A CN105692602A CN 105692602 A CN105692602 A CN 105692602A CN 201610129739 A CN201610129739 A CN 201610129739A CN 105692602 A CN105692602 A CN 105692602A
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C01P2002/00—Crystal-structural characteristics
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention relates to a method for simply and rapidly preparing thin graphene. The method comprises steps as follows: a, a graphite raw material is put in a beaker, ammonium persulfate and concentrated sulfuric acid are added to the beaker, the mixture is stirred, hydrogen peroxide is added, and the mixture is left to stand, washed with water and then dried; b, an oxidizing agent, concentrated sulfuric acid and a dried product obtained in the step a are taken, put in the beaker, stirred, washed with distilled water and diluted hydrochloric acid alternately and centrifuged; c, distilled water is added to the centrifuged product obtained in the step b, an intercalator is added, and the mixture is subjected to ultrasonic treatment and cleaned with ethanol; d, a reducer is added to a water solution of the cleaned product obtained in the step c, the mixture is stirred for sufficient reduction, cooled to the room temperature, alternately washed with deionized water and ethanol and dried, and the thin graphene is obtained. The method is simple to operate, the period is greatly shortened, the production efficiency is high, and the second-cycle reversible specific discharge capacity of the prepared graphene can reach 1,015.8 mAh/g and is higher than the standard theoretical specific capacity of graphene (540 mAh/g).
Description
Technical field
The present invention relates to a kind of method that simple and fast prepares thin graphene, particularly a kind of method preparing thin graphene by slight oxidation and intercalation, belongs to new carbon technical field。
Background technology
Lithium secondary battery has the advantages such as high-energy-density, high working voltage and long-life, has been widely used for the portable electronics such as mobile phone, notebook computer。But the burn event because short circuit causes occurred in the application due to lithium secondary battery, and lithium metal was prone to ignition because character is active, thus have impact on application。For this, work out the lithium ion battery making negative pole carrier with carbon body etc., make the problems referred to above be avoided, it has also become secondary cell with the fastest developing speed。Along with the continuous raising that the indices of energy storage device is required by practical application, current energy storage device cannot practical requirement。The domain requirement degree such as automobile, electronics, communication, military affairs, Aero-Space, medical treatment are also increasing, it is desirable to also more and more higher。But, conventional lithium ion battery material existing defects, for instance, charging interval length, power density are relatively low。In some high impulses are applied, conventional lithium ion battery material is difficult to meet the high power required for system and energy storage density。
Graphene (graphene) is a kind of by monolayer bi-dimensional cellular shape (the only including hexagonal primitive unit cell) lattice structure of the tightly packed one-tenth of carbon atom, and it is by sp2The mono-layer graphite sheet of the carbon atom close-packed arrays of hydridization, this graphite flake has higher specific surface area, prominent heat conductivility and mechanical property so that it is can as the electrode material of the energy storage devices such as lithium ion battery, ultracapacitor, solaode and fuel cell in energy storage field。But, current great majority are prepared the technique of Graphene and be there is complex operation, severe reaction conditions, cause that cost is high, poor product quality。Such as, Graphene perfect crystalline prepared by chemical vapour deposition technique (CVD), large area, high-quality, but cost is high, complex process, substrate requirement condition high；Although graphite oxide method of reducing prepares Graphene simplicity, low cost, but there is more defect in the Graphene of preparation；Graphene quality prepared by epitaxial growth method is high, but prepares the in uneven thickness of Graphene, and the requirement of the equipment of production is high。Therefore, simple for technique, can quickly produce the grapheme material that the number of plies is few, defect is little, increasingly come into one's own。
Summary of the invention
It is an object of the invention to overcome the defect existed in existing graphene preparation method, provide a kind of method that simple and fast prepares thin graphene, it is not only simple to operate that the method prepares Graphene, cycle is greatly shortened, the strong oxidizer kind and the quantity that use are few, production efficiency is high, and products therefrom can keep the conjugated structure of Graphene, reduces the fault of construction of thin graphene。
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that。
The method that a kind of simple and fast of the present invention prepares thin graphene, the method detailed process and step be:
A. take 0.05～1g graphite raw material and put in beaker, be added thereto to 0.1～1.5g Ammonium persulfate. and 1～10mL concentrated sulphuric acid, stir 50min, be slowly added to 1～5mL hydrogen peroxide wherein, stand 2-24h, expand, with deionized water wash, filtration, 60 DEG C of dry 8h；
B. the dried product taking oxidant 0.05～3g, concentrated sulphuric acid 1～10mL and above-mentioned steps a gained is put in beaker, stirs 30～180min, after stirring, with distilled water and the centrifugal 5Min of dilute hydrochloric acid alternately washing；
C. in the centrifugal product of the washing of above-mentioned steps b gained, add distilled water, add 1～5mL intercalator, ultrasonic 0.5～5h under the power of 100w, then uses ethanol purge；
D. in the aqueous solution of the product after the cleaning of step c gained, add 0.1～5mL reducing agent, at 70～100 DEG C, stir 1～5h, fully reduction, after being cooled to room temperature, with 40ml deionized water and the alternately washing of 40ml ethanol, dry 8-24h, can obtain thin graphene after drying。
Graphite described in above-mentioned steps a is the one in native graphite, flaky graphite or expanded graphite。
Oxidant described in above-mentioned steps b is the one in potassium ferrate, Na2Fe04 or potassium permanganate。
Intercalator described in above-mentioned steps c is the one in phenethylamine, aniline or benzylamine。
Reducing agent described in above-mentioned steps d is the one in the aqueous solution of hydrazine hydrate, sodium borohydride, hydroiodic acid, citric acid or glucose。
Compared with the existing technology, the inventive method has following apparent prominent substantive distinguishing features and has the remarkable advantages that:
(1). preparation technology of the present invention is simple, in preparation process, operates at normal temperatures, and manufacturing cycle is short, and efficiency is high, can scale application；In preparation process, the required strong oxidizer kind used is few, quantity is few, it is to avoid use the experimental apparatus that structure is more complicated, large-scale；
(2). the present invention prepares in Graphene process: graphite raw material partial oxidation and fully reduce, remain the structure of Graphene, reduce its oxygen content；Intercalation in preparation process adopts the form of a kind of " molecule shovel " to peel off graphite linings, decreases the fault of construction of Graphene。
(3). grapheme material prepared by the preparation method of the present invention, its chemical property is improved, under 50mA/g electric current density, first discharge specific capacity is 1946mAh/g, 2nd circulating and reversible specific discharge capacity is up to 1015.8mAh/g, higher than the theoretical specific capacity (540mAh/g) of Graphene standard。
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of thin graphene prepared by the inventive method。
Fig. 2 is the SEM figure of thin graphene prepared by the inventive method。
Fig. 3 is the TEM figure of thin graphene prepared by the inventive method。
Fig. 4 is the charging and discharging curve figure of thin graphene prepared by the inventive method。
Detailed description of the invention
Further illustrate method provided by the present invention by the examples below。
Embodiment 1
A kind of simple and fast prepares the method for thin graphene, and the step of the method is as follows:
1). take 0.5g (NH4)2S2O8Put in 50mL beaker with 6mL concentrated sulphuric acid and 0.1g native graphite, after stirring 50min, be slowly added to the 30% hydrogen peroxide (H of 2mL wherein2O2), stand 5h, expand, with deionized water wash, filter, at 60 DEG C of dry 8h；
2). the dried product taking Na2Fe04 0.05g, concentrated sulphuric acid 5mL and above-mentioned steps 1 gained is put in beaker, stirs 90min, with distilled water diluting after stirring, stands, pours out supernatant；With 5min centrifugal under dilute hydrochloric acid washing, 5000r/min；
3). by centrifugal for the washing of step 2 gained product adds distilled water 400mL, add 2mL phenethylamine, ultrasonic 1h under the power of 100w, then wash away phenethylamine with ethanol；
4). in the aqueous solution of the product after the cleaning of step 3 gained, add 0.1mL hydrazine hydrate, at 80 DEG C, stir 2h, fully reduce, after being cooled to the alternately washing 3 times of room temperature, deionized water and ethanol, at-40 DEG C of lyophilization 24h, thin graphene can be obtained。
The test of the thin graphene electrical property prepared:
By the product of preparation through cal rolling flakiness, blunderbuss becomes pole piece to be pressed on copper mesh, obtains working electrode, with metal lithium sheet for negative pole, with microporous polypropylene membrane for barrier film, with 1mol/L hexafluoro phosphatization lithium (LiPF6) diethyl carbonate (DEC) and the solution that is made into of dimethyl carbonate (DMC) solution (volume ratio 1:1) be electrolyte, the glove box of full argon assembles CR2032 type button graphene battery, carry out constant current charge-discharge test, through can be calculated the specific capacitance of single electrode of material。
As shown in Figure 1, as seen from the figure, the Graphene of preparation disordering, without obvious crystalline structure, also without obvious impurity peaks for the XRD of product。Fig. 2 and Fig. 3 is scanning electron microscope (SEM) and transmission electron microscope (TEM) photo of the Graphene prepared respectively, finds out in the appearance structure from Fig. 2 and Fig. 3, and graphite is stripped into thin layer。The charging and discharging curve of the Graphene from Fig. 4 is it can be seen that the first discharge specific capacity under 50mA/g electric current density is up to 1946mAh/g, and the reversible specific capacity of the 2nd circulation electric discharge, up to 1015.8mAh/g, has good cycle performance。
Embodiment 2
1). take 0.2g (NH4)2S2O8Put in 30mL beaker with 1mL concentrated sulphuric acid and 0.05g flaky graphite, after stirring 50min, be slowly added to the 30% hydrogen peroxide (H of 1mL wherein2O2), stand 2h, fully expand, with deionized water wash, filter, at 60 DEG C of dry 8h；
2). the dried product taking potassium permanganate 0.75g, concentrated sulphuric acid 4mL and above-mentioned steps 1 gained is put in beaker, stirs 90min, with distilled water diluting after stirring, stands, pours out supernatant；With 5min centrifugal under dilute hydrochloric acid washing, 5000r/min；
3). by centrifugal for the washing of step 2 gained product adds distilled water 200mL, add 1mL aniline, ultrasonic 3h under the power of 100w, then alternately cleans with ethanol and deionized water；
4). in the aqueous solution of the product after the cleaning of step 3 gained, add 1mL sodium borohydride solution, at 70 DEG C, stir 5h, fully reduction, after being cooled to the alternately washing 3 times of room temperature, deionized water and ethanol, at-60 DEG C of lyophilization 24h, thin graphene can be obtained。
What the present embodiment 2 prepared thin graphene electric performance test method is with embodiment 1, and the first discharge specific capacity recorded through electro-chemical test of preparation is 1800mAh/g, and the reversible specific capacity of the 2nd circulation electric discharge is up to 986.7mAh/g。
Embodiment 3
1). take 1.0g (NH4)2S2O8Put in 250mL beaker with 10mL concentrated sulphuric acid and 1.0g expanded graphite, after stirring 50min, be slowly added to the 30% hydrogen peroxide (H of 3mL wherein2O2), stand 24h, fully expand, with deionized water wash, filter, at 60 DEG C of dry 8h；
2). the dried product taking potassium ferrate 3.0g, concentrated sulphuric acid 8mL and above-mentioned steps 1 gained is put in beaker, stirs 120min, with distilled water diluting after stirring, stands, pours out supernatant；With 5min centrifugal under dilute hydrochloric acid washing, 5000r/min。
3). by centrifugal for the washing of step 2 gained product adds distilled water 1500mL, add 5mL phenethylamine, ultrasonic 5h under the power of 100w, then alternately cleans with ethanol and deionized water；
4). in the aqueous solution of the product after the cleaning of 3 step gained, add 2mL hydroiodic acid, at 100 DEG C, stir 1h, fully reduce, after being cooled to the alternately washing 3 times of room temperature, deionized water and ethanol, vacuum drying 12h, thin graphene can be obtained。
What the present embodiment 3 prepared thin graphene electric performance test method is with embodiment 1, and the specific capacity recorded through electro-chemical test of preparation is 1680mAh/g, and the reversible specific capacity of the 2nd circulation electric discharge is up to 1051.9mAh/g。
Embodiment 4
1). take 1.5g (NH4)2S2O8Put in 50mL beaker with 8mL concentrated sulphuric acid and 0.3g native graphite, after stirring 50min, be slowly added to the 30% hydrogen peroxide (H of 5mL wherein2O2), stand 15h, fully expand, with deionized water wash, filter, at 60 DEG C of dry 8h；
2). the dried product taking potassium ferrate 1.3g, concentrated sulphuric acid 1mL and above-mentioned steps 1 gained is put in beaker, stirs 180min, with distilled water diluting after stirring, stands, pours out supernatant；Again with 5min centrifugal under dilute hydrochloric acid washing, 5000r/min；
3). by centrifugal for the washing of step 2 gained product adds distilled water 800mL, add 4mL aniline, ultrasonic 0.5h under the power of 100w, then uses ethanol purge；
4). the aqueous solution of the product after the cleaning of step 3 gained adds 3mL citric acid, at 70 DEG C, stirs 2h, fully reduce, after being cooled to the alternately washing 3 times of room temperature, deionized water and ethanol, vacuum drying 8h, thin graphene can be obtained。
What the present embodiment 4 prepared thin graphene electric performance test method is with embodiment 1, and the specific capacity recorded through electro-chemical test of preparation is 1760mAh/g, and the reversible specific capacity of the 2nd circulation electric discharge is up to 1034.3mAh/g。
Embodiment 5
1). take 0.1g (NH4)2S2O8Put in 300mL beaker with 4mL concentrated sulphuric acid and 0.2g expanded graphite, after stirring 50min, be slowly added to the 30% hydrogen peroxide (H of 4mL wherein2O2), stand 10h, fully expand, with deionized water wash, filter, at 60 DEG C of dry 8h；
2). the dried product taking potassium permanganate 2.2g, concentrated sulphuric acid 10mL and above-mentioned steps 1 gained is put in beaker, stirs 30min, with distilled water diluting after stirring, stands, pours out supernatant；With 5min centrifugal under dilute hydrochloric acid washing, 5000r/min；
3). by centrifugal for the washing of step 2 gained product adds distilled water 500mL, add 2.5mL benzylamine, ultrasonic 5h under the power of 100w, then alternately cleans with ethanol and deionized water；
4). the aqueous solution of the product after the cleaning of step 3 gained adds the aqueous solution of 5mL glucose, at 80 DEG C, stirs 4h, fully reduce, it is cooled to room temperature, after deionized water and ethanol alternately wash 3 times, air dry oven dries about 24h, can obtain thin graphene。
What the present embodiment 5 prepared thin graphene electric performance test method is with embodiment 1, and the material of preparation is 1660mAh/g through the specific capacity that electro-chemical test records, and the reversible specific capacity of the 2nd circulation electric discharge is up to 1121.6mAh/g。
Claims (5)
1. the method that simple and fast prepares thin graphene, the method detailed process and step be:
A. take 0.05～1g graphite raw material and put in beaker, be added thereto to 0.1～1.5g Ammonium persulfate. and 1～10mL concentrated sulphuric acid, stir 50min, be slowly added to 1～5mL hydrogen peroxide wherein, stand 2-24h, expand, with deionized water wash, filtration, 60 DEG C of dry 8h；
B. the dried product taking oxidant 0.05～3g, concentrated sulphuric acid 1～10mL and above-mentioned steps a gained is put in beaker, stirs 30～180min, after stirring, with distilled water and the centrifugal 5Min of dilute hydrochloric acid alternately washing；
C. in the centrifugal product of the washing of above-mentioned steps b gained, add distilled water, add 1～5mL intercalator, ultrasonic 0.5～5h under the power of 100w, then uses ethanol purge；
D. in the aqueous solution of the product after the cleaning of step c gained, add 0.1～5mL reducing agent, at 70～100 DEG C, stir 1～5h, fully reduction, after being cooled to room temperature, with 40ml deionized water and the alternately washing of 40ml ethanol, dry 8-24h, can obtain thin graphene after drying。
2. the method that a kind of simple and fast according to claim 1 prepares thin graphene, it is characterised in that the graphite described in above-mentioned steps a is the one in native graphite, flaky graphite or expanded graphite。
3. the method that a kind of simple and fast according to claim 1 prepares thin graphene, it is characterised in that the oxidant described in above-mentioned steps b is the one in potassium ferrate, Na2Fe04 or potassium permanganate。
4. the method that a kind of simple and fast according to claim 1 prepares thin graphene, it is characterised in that the intercalator described in above-mentioned steps c is the one in phenethylamine, aniline or benzylamine。
5. the method that a kind of simple and fast according to claim 1 prepares thin graphene, it is characterised in that the reducing agent described in above-mentioned steps d is the one in the aqueous solution of hydrazine hydrate, sodium borohydride, hydroiodic acid, citric acid or glucose。
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Cited By (7)
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| CN107827097A (en) * | 2017-11-22 | 2018-03-23 | 四川大学 | A kind of graphene synthetic method without external energy input |
| CN108101035A (en) * | 2018-03-06 | 2018-06-01 | 绍兴文理学院 | A kind of environment-friendly preparation method thereof of high-quality graphene |
| CN108285143A (en) * | 2018-01-24 | 2018-07-17 | 江苏理工学院 | A kind of preparation method of biomass-based N doping thin layer graphite carbon material |
| CN109499497A (en) * | 2019-01-03 | 2019-03-22 | 太原理工大学 | A kind of preparation method of graphene/carbon microballoon composite aerogel |
| CN111204743A (en) * | 2020-02-07 | 2020-05-29 | 西南交通大学 | Method for preparing twisted graphene by utilizing polymer spiral growth |
| CN114709083A (en) * | 2022-05-25 | 2022-07-05 | 深圳市今朝时代股份有限公司 | Modified graphene composite material and supercapacitor |
| CN115448298A (en) * | 2022-09-26 | 2022-12-09 | 天津市职业大学 | High-efficiency transposition washing method for preparing thin-layer graphene |
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| CN108101035A (en) * | 2018-03-06 | 2018-06-01 | 绍兴文理学院 | A kind of environment-friendly preparation method thereof of high-quality graphene |
| CN109499497A (en) * | 2019-01-03 | 2019-03-22 | 太原理工大学 | A kind of preparation method of graphene/carbon microballoon composite aerogel |
| CN109499497B (en) * | 2019-01-03 | 2021-03-16 | 太原理工大学 | Preparation method of graphene/carbon microsphere composite aerogel |
| CN111204743A (en) * | 2020-02-07 | 2020-05-29 | 西南交通大学 | Method for preparing twisted graphene by utilizing polymer spiral growth |
| CN111204743B (en) * | 2020-02-07 | 2023-02-07 | 西南交通大学 | Method for preparing twisted graphene by utilizing polymer spiral growth |
| CN114709083A (en) * | 2022-05-25 | 2022-07-05 | 深圳市今朝时代股份有限公司 | Modified graphene composite material and supercapacitor |
| CN114709083B (en) * | 2022-05-25 | 2022-10-25 | 深圳市今朝时代股份有限公司 | Modified graphene composite material and supercapacitor |
| CN115448298A (en) * | 2022-09-26 | 2022-12-09 | 天津市职业大学 | High-efficiency transposition washing method for preparing thin-layer graphene |
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Application publication date: 20160622 |