CN102464315A - Preparation method of graphene - Google Patents
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- CN102464315A CN102464315A CN201010548936XA CN201010548936A CN102464315A CN 102464315 A CN102464315 A CN 102464315A CN 201010548936X A CN201010548936X A CN 201010548936XA CN 201010548936 A CN201010548936 A CN 201010548936A CN 102464315 A CN102464315 A CN 102464315A
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Abstract
The invention relates to a preparation method of graphene, comprising the following steps of: heating expandable graphite in protective atmosphere, and thermally stripping to obtain expanded graphite; dissolving the expanded graphite into solution containing a surfactant, and ultrasonically stripping to obtain graphene solution; centrifuging, filtering, washing and drying the graphene solution in sequence so as to obtain a crude graphene product; and performing a microwave heating treatment to the crude graphene product to obtain the graphene. The preparation method of the graphene has the advantages of lower cost and higher purity.
Description
[technical field]
The invention belongs to the organic semiconductor material technical field, be specifically related to a kind of preparation method of graphene.
[background technology]
Prepared grapheme material in 2004 since the strong K of the peace moral of Univ Manchester UK sea nurse (Andre K.Geim) waits, pay attention to widely owing to its particular structure and photoelectric property have received people.Mono-layer graphite is because its big specific surface area, good conduction, heat conductivility and low thermal expansivity and be considered to desirable material.As: 1. HS, Young's modulus, (1,100GPa), breaking tenacity: (125GPa); 2. high heat conductance, (5,000W/mK); 3. high conductivity, carrier transport rate, (200,000cm
2/ Vs); 4. high specific surface area, (calculated value: 2,630m
2/ g).Especially its high conductivity matter, the textural property of the big specific surface character and the nanoscale of its unimolecular layer two dimension can be used as electrode materials in ultracapacitor and lithium ion battery.
Up to the present, the known method for preparing Graphene has following several kinds: (1) micromechanics is peeled off 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) oxidation-reduction method.Whole process relates to graphite oxidation is become graphite oxide, and graphite oxide peels off the graphene oxide of generation, is Graphene through chemistry or thermal reduction again.This method synthetic Graphene is easier to produce defective (4) chemical Vapor deposition process (CVD).This method can satisfy the requirement of scale preparation high quality Graphene, but cost is higher, complex process.(5) solvent is peeled off method.This method shortcoming is that productive rate is very low, limits its commercial applications; (6) electrolytic process.This method can be synthesized a large amount of Graphenes, but the surface of the Graphene that synthesizes all has a large amount of positive ions or negative ion or organism.(7) solvent-thermal method.This method synthetic Graphene purity is higher, but the reaction times is longer relatively, and productive rate has only 1%～5%.
[summary of the invention]
Based on this, be necessary to provide that a kind of cost is lower, purity and the higher preparation method of graphene of productive rate.
A kind of preparation method of graphene comprises the steps: heating expansible black lead under protective atmosphere, obtains expanded graphite after hot soarfing leaves; Said expanded graphite is dissolved in the solution that contains tensio-active agent, and ultrasonic peeling off obtains Graphene solution; Said Graphene solution is carried out centrifugal, filtration, washing and drying treatment successively, obtain the thick product of Graphene; And the thick product of said Graphene is carried out microwave heating treatment, obtain Graphene.
In preferred embodiment, the median size of expansible black lead is 300～500 μ m, and purity is 99～99.5%.
In preferred embodiment, Heating temperature is 800 ℃～1200 ℃, and the time is 10 seconds～60 seconds.
In preferred embodiment, the microwave reactor that uses 500～1500W was with this expansible black lead heating 10 seconds～5 minutes.
In preferred embodiment, tensio-active agent is an X 2073, at least a in cetyl trimethylammonium bromide, sodium lauryl sulphate, polyoxyethylene octyl phenyl ether, the dioctyl sodium sulfosuccinate.
In preferred embodiment, the concentration of surfactant soln is 5g/L～10g/L.
In preferred embodiment, the concentration of Graphene solution is 0.05g/L～0.1g/L.
In preferred embodiment, ultrasonic strip step is for to leave standstill the said solution supersound process that is dissolved with expanded graphite 12 hours～24 hours after 20 minutes～40 minutes.
In preferred embodiment, also comprise step with the thick product repeating step two of Graphene to step 3.
In preferred embodiment, the power of microwave heating treatment is 500W～1500W, and be 60 seconds～120 seconds heat-up time.
Above-mentioned preparing method's advantage is: 1. adopt expanded graphite as starting material, the low price cost is low, is prone to peel off into Graphene, and can improve productive rate greatly; 2. adopt water and tensio-active agent to peel off reagent, safer, environmental protection and environmental friendliness as intercalation; 3. pass through the microwave heating treatment of step 4, can water molecules in the Graphene and tensio-active agent be removed, obtain highly purified Graphene; 4. the equipment that adopts is simple, easy to operate, and production stage is few, is suitable for scale operation; Parameters such as the power that 5. heats through controlled microwave, time can easily be adjusted the strong and weak degree to the thick product treatment of Graphene.In addition, the microwave equipment start-stop is convenient, has efficient and energy-saving advantages.
[description of drawings]
Fig. 1 is the schema of the preparation method of graphene of an embodiment.
Fig. 2 is the SEM figure of the Graphene for preparing among the embodiment.
[embodiment]
To combine accompanying drawing and embodiment that preparation method of graphene is done further to specify below.
See also Fig. 1, the preparation method of graphene of an embodiment comprises the steps:
Step S101 provides expansible black lead.This expansible black lead is the expansible black lead that meets GB GB/T 10698-1989, becomes vermiform natural crystalloid graphite but refer generally to after special processing, meet the high temperature instantaneous expansion.The mean diameter of the employed expansible black lead of this embodiment is 300～500 μ m, and purity is 99～99.5%.
Step S102, this expansible black lead of heating obtains expanded graphite after hot soarfing leaves under protective atmosphere.In this embodiment, expansible black lead is being fed hybrid protection gas (2%～7%H
2Under 93%～98%Ar) condition, be heated to 800 ℃～1200 ℃, the treatment time is 10s～60s (second), and expansible black lead is expanded, and carries out hot soarfing then and leaves, and obtains expanded graphite.Certainly, also can adopt N
2Wait other shielding gas.In addition, can also be under protective atmosphere, the microwave reactor that uses 500～1500W with this expansible black lead heating 10s (second)～5min (minute), make the expansible black lead expansion, carry out hot soarfing then and leave, obtain expanded graphite.
Step S103 is dissolved into the expansible black lead after the heating in the solution that contains tensio-active agent, and ultrasonic peeling off obtains Graphene solution; In this embodiment, expanded graphite is joined in the aqueous solution that contains tensio-active agent that concentration is 5～10g/L, through supersound process 20～40min, leave standstill 10～24h (hour) after, obtaining concentration is the Graphene solution of 0.05～0.1g/L.That tensio-active agent has is wetting or anti-stick, emulsification or breakdown of emulsion, foaming or froth breaking and solubilising, dispersion, washing, a series of physics chemical action such as anticorrosion, antistatic.In this embodiment, the main effect of tensio-active agent is to make Graphene well scatter, and the purpose of water is exactly that intercalation is peeled off, and makes expanded graphite peel off into Graphene.Tensio-active agent can be selected X 2073 (SDBS) for use, cetyl trimethylammonium bromide, sodium lauryl sulphate, polyoxyethylene octyl phenyl ether, dioctyl sodium sulfosuccinate etc.
Step S104 carries out centrifugal, filtration, washing and drying treatment successively with Graphene solution, obtains the thick product of Graphene.In this embodiment; At first this Graphene solution centrifugal is separated, supernatant is collected, filtered, clean repeatedly with deionized water and ethanol then; Last in vacuum drying oven with 80～100 ℃ temperature drying 2～5 hours, promptly obtain the thick product of Graphene.
In preferred embodiment, also comprise the processing of the thick product of Graphene being carried out again step S103 to S104 repeatedly, to improve thick yield of product of Graphene and purity.
Step S105, the thick product of Graphene that step S104 is obtained carries out microwave heating treatment, obtains Graphene.In this embodiment, the thick product of Graphene that step S104 obtains is put into microwave reactor, regulating microwave power is 500～1500W, and heating 60～120s removing water molecules and tensio-active agent, thereby obtains highly purified Graphene.
Above-mentioned preparing method's advantage is: 1. adopt expanded graphite as starting material, the low price cost is low, is prone to peel off into Graphene, and can improve productive rate greatly; 2. adopt water and tensio-active agent to peel off reagent, safer, environmental protection and environmentally friendly as intercalation; 3. pass through the microwave heating treatment of step 4, can water molecules in the Graphene and tensio-active agent be removed, obtain highly purified Graphene; 4. the equipment that adopts is simple, easy to operate, and production stage is few, is suitable for scale operation; Parameters such as the power that 5. heats through controlled microwave, time can easily be adjusted the strong and weak degree to the thick product treatment of Graphene.In addition, the microwave equipment start-stop is convenient, has efficient and energy-saving advantages.
Institute's synthetic Graphene as electrode materials can use with ultracapacitor in.
Describe below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of high purity graphite alkene, its technical process is following:
(1) provide mean diameter 300 μ m, the expansible black lead of purity 99%;
(2) expansible black lead is being fed hybrid protection gas (5%H
2And 95%Ar) under the condition, be heated to 800 ℃ and handle 60s, hot soarfing forms expanded graphite from the back;
(3) expanded graphite (25mg) in (2) is joined 250ml, concentration is in the X 2073 solution of 5mg/ml, behind the ultrasonic 30min, leaves standstill 12h, and ultrasonic peeling off forms Graphene solution;
(4) the Graphene solution in (3) was carried out centrifugal 30 minutes, supernatant is collected, filter, clean repeatedly with deionized water and ethanol, at last in vacuum drying oven with 80 ℃ of dry 2h, obtain the thick product of Graphene.
(5) microwave reactor of the thick product of Graphene in (4) being put into 1500W heats 60s, removes water molecules and tensio-active agent, obtains highly purified Graphene.
Embodiment 2
A kind of preparation method of high purity graphite alkene, its technical process is following:
(1) provide mean diameter 400 μ m, the expansible black lead of purity 99.5%;
(2) expansible black lead is being fed mixed gas (5%H
2And 95%Ar) under the condition, is heated to 1200 ℃ and handles 10s, form expanded graphite;
(3) expanded graphite (25mg) in (2) is joined 500ml, concentration is in the cetyl trimethylammonium bromide solution of 50mg/ml, behind the ultrasonic 30min, leaves standstill 24h, and ultrasonic peeling off forms Graphene solution;
(4) the Graphene solution in (3) is carried out centrifugal 30min, supernatant is collected, filter, clean repeatedly with deionized water and ethanol, at last in vacuum drying oven with 80 ℃ of dry 2h, obtain the thick product of Graphene.
(5) throw out after centrifugal is repeated the operation of (3)～(4) again, obtain the thick yield of product of Graphene with raising.
(6) the thick product of Graphene in (5) is put into the microwave reactor heating 120 seconds of 500W, removed water molecules and tensio-active agent, obtain highly purified Graphene.
Embodiment 3
A kind of preparation method of high purity graphite alkene, its technical process is following:
(1) provide mean diameter 500 μ m, the expansible black lead of purity 99%;
(2) expansible black lead is reacted 10s in the 1500W microwave reactor after, hot soarfing is from obtaining expanded graphite;
(3) expanded graphite (25mg) in (2) is joined 250ml, concentration is in the sodium dodecyl sulfate solution of 5mg/ml, behind the ultrasonic 30min, leaves standstill 12h, and ultrasonic peeling off forms Graphene solution;
(4) the Graphene solution in (3) was carried out centrifugal 30 minutes, supernatant is collected, filter, clean repeatedly with deionized water and ethanol, at last in vacuum drying oven with 80 ℃ of dry 2h, obtain the thick product of Graphene.
(5) microwave reactor of the thick product of Graphene in (4) being put into 600W heats 60s, removes water molecules and tensio-active agent, obtains highly purified Graphene.
Embodiment 4
A kind of preparation method of high purity graphite alkene, its technical process is following:
(1) provide mean diameter 400 μ m, the expansible black lead of purity 99%;
(2) expansible black lead is reacted 5 minutes in the 500W microwave reactor after, hot soarfing is from obtaining expanded graphite;
(3) expanded graphite (25mg) in (2) is joined 250ml, concentration is in the polyoxyethylene octyl phenyl ether solution of 10mg/ml, behind the ultrasonic 30min, leaves standstill 12h, and ultrasonic peeling off forms Graphene solution;
(4) the Graphene solution in (3) is carried out centrifugal 30min, supernatant is collected, filter, clean repeatedly with deionized water and ethanol, at last in vacuum drying oven with 80 ℃ of dry 2h, obtain the thick product of Graphene.
(5) throw out after centrifugal is repeated the operation of (3)～(4) again, obtain the thick yield of product of Graphene with raising.
(6) the thick product of Graphene in (5) is put into the microwave reactor heating 60 seconds of 600W, removed water molecules and tensio-active agent, obtain highly purified Graphene.
See also Fig. 2, be depicted as ESEM (SEM) collection of illustrative plates of the Graphene of embodiment 1 preparation.Can know that by Fig. 2 this method can access the higher Graphene product of purity, and this Graphene product has good sheet structure.
The above embodiment has only expressed several kinds of embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the present invention's design, 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 accompanying claims.
Claims (10)
1. a preparation method of graphene is characterized in that, comprises the steps:
Step 1, under protective atmosphere the heating expansible black lead, obtain expanded graphite after hot soarfing leaves;
Step 2, said expanded graphite is dissolved in the solution that contains tensio-active agent, ultrasonic peeling off obtains Graphene solution;
Step 3, said Graphene solution is carried out centrifugal, filtration, washing and drying treatment successively, obtain the thick product of Graphene; And
Step 4, the thick product of said Graphene is carried out microwave heating treatment, obtain Graphene.
2. preparation method of graphene according to claim 1 is characterized in that: the median size of expansible black lead is 300～500 μ m in the said step 1, and purity is 99～99.5%.
3. preparation method of graphene according to claim 1 is characterized in that: Heating temperature is 800 ℃～1200 ℃ in the said step 1, and the time is 10 seconds～60 seconds.
4. preparation method of graphene according to claim 1 is characterized in that: said step 1 heats this expansible black lead 10 seconds～5 minutes for the microwave reactor that uses 500～1500W.
5. preparation method of graphene according to claim 1; It is characterized in that: tensio-active agent is an X 2073 in the said step 2, at least a in cetyl trimethylammonium bromide, sodium lauryl sulphate, polyoxyethylene octyl phenyl ether, the dioctyl sodium sulfosuccinate.
6. preparation method of graphene according to claim 5 is characterized in that: the concentration of said surfactant soln is 5g/L～10g/L.
7. preparation method of graphene according to claim 1 is characterized in that: the concentration of Graphene solution is 0.05g/L～0.1g/L in the said step 2.
8. preparation method of graphene according to claim 1 is characterized in that: ultrasonic strip step is for to leave standstill the said solution supersound process that is dissolved with expanded graphite 12 hours～24 hours in the said step 2 after 20 minutes～40 minutes.
9. preparation method of graphene according to claim 1 is characterized in that: the step that also comprises the thick product repeating step two of the Graphene that said step 3 is obtained to step 3 before the said step 4.
10. preparation method of graphene according to claim 1 is characterized in that: the power of microwave heating treatment is 500W～1500W in the said step 4, and be 60 seconds～120 seconds heat-up time.
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| CN103435033A (en) * | 2013-08-12 | 2013-12-11 | 上海理工大学 | Simple and convenient method for preparing graphene-zinc oxide nanorod composite material in ultrasonic wave |
| CN103449414A (en) * | 2012-05-31 | 2013-12-18 | 海洋王照明科技股份有限公司 | Preparation method of graphene having porous structure |
| CN103466605A (en) * | 2013-08-22 | 2013-12-25 | 广东工业大学 | Preparation method of nano graphite sheet |
| CN103803532A (en) * | 2012-11-15 | 2014-05-21 | 福建省辉锐材料科技有限公司 | Preparation method of high thermal conductivity graphene thin film |
| CN103803533A (en) * | 2012-11-15 | 2014-05-21 | 福建省辉锐材料科技有限公司 | Preparation method of graphene |
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| CN105110326A (en) * | 2015-09-10 | 2015-12-02 | 朱振业 | Method adopting a liquid phase stripping method to prepare grapheme and grapheme |
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Application publication date: 20120523 |