CN105967181A - Graphene and preparation method thereof - Google Patents
Graphene and preparation method thereof Download PDFInfo
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- CN105967181A CN105967181A CN201610578062.XA CN201610578062A CN105967181A CN 105967181 A CN105967181 A CN 105967181A CN 201610578062 A CN201610578062 A CN 201610578062A CN 105967181 A CN105967181 A CN 105967181A
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- graphene
- preparation
- thermal reduction
- dialysis
- graphene oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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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
Abstract
The invention relates to the field of graphene and particularly relates to a preparation method of the graphene. The preparation method comprises the following steps: providing graphene oxide; dialyzing the graphene oxide; cooling and drying; carrying out thermal reduction; and finally, carrying out chemical reduction to obtain the graphene. According to the preparation method of the graphene, relatively a few of graphene sheets are obtained through steps of dialyzing, freeze drying, firstly carrying out the thermal reduction and then carrying out the chemical reduction and the like; and a graphene product is formed by piling up relatively few layers of carbon atoms which are periodically and tightly stacked as a benzene ring structure (namely a hexagonal honeycomb structure) and the quality of the graphene is relatively high. Furthermore, the preparation method provided by the invention is conventional in raw materials and relatively low in cost; and needed equipment is simple, the up-front cost is relatively low and the manufacturing cost can be effectively reduced. The invention further discloses the graphene obtained by the preparation method.
Description
Technical field
The present invention relates to field of graphene, particularly relate to a kind of Graphene and preparation method thereof.
Background technology
Graphene (English name Graphene) is a kind of cellular quasi-two-dimensional structure formed by carbon atom.
Graphene is the basic structural unit of all carbon crystals in addition to diamond.Graphene has the two dimension of almost Perfect
Crystal structure, its lattice is the hexagon surrounded by six carbon atom, thickness only one of which carbon atomic layer
Thickness.Being that s is bonded between atom, combination is sp2Hydridization.Additionally Graphene has the electron energy band of uniqueness
Structure, the effective mass in Graphene is zero.These features make Graphene have high-specific surface area (2620
m2·g-1), high charge mobility electrically (25000cm2·V-1·s-1), high structural strength (1TPa) and high heat
Conductivity (5000W m-1·K-1) etc. characteristic.Due to above-mentioned characteristic, the application prospect of Graphene is very wide, from
Single-electronic transistor, bipolarity transistor, flexible transistor, electrode material of lithium battery, super capacitor electrode
Material, solaode window electrode to transmission line of electricity and space elevator have application.
At present, Graphene has multiple preparation method, including mechanical stripping method, graphite oxide reducing process,
Surface epitaxial growth method and chemical vapour deposition technique etc..Wherein, current surface epitaxial growth method and chemistry
Vapour deposition process is unfavorable for large-scale production；At present the most ripe and can aoxidize with scale of mass production
Graphite reduction method and mechanical stripping method.But, current above two method, obtain quality of graphene relatively low.
Summary of the invention
Based on this, it is necessary to in prior art, the graphene preparation method that can be mass-produced, obtain
The relatively low problem of quality of graphene, it is provided that a kind of quality is high and the preparation side of Graphene that can be mass-produced
Method.
The preparation method of a kind of Graphene, it is characterised in that comprise the steps:
Graphene oxide is provided；
Described graphene oxide is dialysed；
Graphene oxide after dialysis is carried out lyophilization；
Graphene oxide after lyophilization is carried out thermal reduction, obtains thermal reduction product；
Described thermal reduction product is carried out electronation, obtains Graphene.
The preparation method of above-mentioned Graphene, owing to after dialysis, lyophilization and first thermal reduction, chemistry is gone back
The step such as former, the graphene sheet layer obtained is less, Graphene product i.e. by the less number of plies with benzene ring structure (i.e.
Hexagonal honeycomb structure) the most closelypacked carbon atom stacking composition, the quality of Graphene is higher.Separately
Outward, preparation method provided by the present invention, its raw material is conventional, and cost is relatively low, and required equipment is simply,
Early investment is relatively low, can effectively reduce manufacturing cost.
Wherein in an embodiment, described electronation is using hydrazine hydrate as reducing agent.
Wherein in an embodiment, the temperature of described thermal reduction is 950～1150 DEG C, and the time is 20～30s.
Wherein in an embodiment, described thermal reduction is carried out under pressure is 8～12MPa.
Wherein in an embodiment, the current-carrying molecular weight of the dialyzer that described dialysis is used is
8000～14000.
Wherein in an embodiment, before described dialysis, also include in boiling water, boil described dialyzer
7～15min.
Wherein in an embodiment, described dialysis is for carry out unidirectional current dialysis at deionized water, and unidirectional current is saturating
The voltage of analysis is 25V, and the time changes deionized water for being not less than 30 days and every day.
Wherein in an embodiment, described cryodesiccated temperature is-50～-70 DEG C, and vacuum is 10～30Pa.
Wherein in an embodiment, described graphene oxide obtains by improving Hummers method.
Present invention also offers a kind of Graphene.
A kind of Graphene, it is obtained by preparation method provided by the present invention.
Above-mentioned Graphene, owing to being obtained by preparation method provided by the present invention, its lamella is less, graphite
The quality of alkene is higher.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the Graphene A1 of embodiment one.
Fig. 2 is the SEM figure of the Graphene B1 of comparative example one.
Fig. 3-6 is the big multiplying power SEM figure of the Graphene A1 of embodiment one.
Fig. 7 is the Raman spectrogram of the Graphene A1 of embodiment one.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with being embodied as
Mode, is further elaborated to the present invention.Should be appreciated that detailed description of the invention described herein
Only in order to explain the present invention, it is not intended to limit the present invention.
The preparation method of a kind of Graphene, comprises the steps:
S1, offer graphene oxide.
Wherein, graphene oxide (graphene oxide is called for short GO) can be prepared with oneself, it is also possible to passes through business
Available from.
Preferably, graphene oxide is prepared by the Hummer method improved.More specifically, the Hummer improved
Method comprises the steps: to join in dry anhydrous reaction vessel graphite and sodium nitrate, is subsequently adding
H2SO4, mix and blend reacts；Then KMnO is added4Continuing stirring ice bath reaction, subsequently water-bath adds
Heat；Being added to by water droplet wherein, oil bath pan stirs；It is subsequently adding H2O2, it is eventually adding HCl solution, obtains
The liquid of graphene oxide.
S2, graphene oxide is dialysed.
Wherein it is preferred to, the dialysis of deionized water unidirectional current is selected in dialysis, and its concrete operations are: by step S1
The liquid seal of the graphene oxide obtained is encapsulated in bag filter (sack being made up of dialyzer), and puts
Enter to fill in the dialysis apparatus of deionized water, make bag filter be positioned at dialysis apparatus two 260 type platinum electrodes it
Between, switch on power and dialyse.
Specifically, the current-carrying molecular weight of bag filter is preferably 8000～14000, more preferably selects model MD44
Bag filter.
In order to optimize the performance of bag filter further, before dialysis, bag filter is placed in boiling water and boils
7～15min.In the present embodiment, in boiling water, preferably boil 10min.
Preferably, the electrodialytic voltage of direct current is 25V, and the time, every day changed deionization in order to be not less than 30 days
Water.
It is highly preferred that dialysis is until electric current is less than 0.005A.I.e. when electric current is less than 0.005A, terminate dialysis
Operation.
After waiting to terminate dialysis, graphene oxide in bag filter is fully washed and is dried.
S3, to dialysis after graphene oxide carry out lyophilization.
Wherein, cryodesiccated concrete steps include: join in deionized water by dry graphene oxide,
And ultrasonic agitation, then freeze, finally put in freeze dryer and be dried.
In step s3, graphene oxide and the proportioning of deionized water are that every 0.1g graphene oxide is joined
30ml～100ml deionized water.More preferably 0.1g graphene oxide joins 50ml deionized water.
Preferably, the temperature of frost is-55 DEG C, more preferably-20 DEG C.The time of frost is preferably 12h～36h,
More preferably 24h.
Preferably, the temperature being dried be-50～-70 DEG C, is more preferably-55 DEG C.Vacuum when being dried is preferably
10～30Pa, more preferably 17Pa.The time being dried is preferably 24～72h, more preferably 48h.
S4, the graphene oxide after lyophilization is carried out thermal reduction, obtain thermal reduction product.
Specifically, thermal reduction step is: first heated by argon stove, when in graphite tube, temperature reaches preset temperature
It is passed through argon after (preferably 950～1150 DEG C), and uses CO2Pressure regulator is transferred to 8～about 12MPa；Then
The corundum crucible being loaded with graphene oxide is put in graphite tube, heats 20～30s, heated and taken out at once,
Sample is prevented to be burned.
It is, of course, understood that thermal reduction step is not limited to above-mentioned steps, those skilled in the art
Can make reasonably to change according to practical situation.
S5, described thermal reduction product is carried out electronation, obtain Graphene.
In step s 5, specifically, ammonia and hydrazine hydrate are joined in the dispersion liquid of thermal reduction product and stir
Reaction.Specifically, magnetic agitation 4h at 80 DEG C.React complete after, sucking filtration final vacuum is dried.
Preferably, before hydrazine hydrate adds, also include thermal reduction product is carried out ultrasonic disperse.More specifically
Ground, adds thermal reduction product in deionized water, ultrasonic 240min.So can be sufficiently mixed and the group of preventing
Poly-.
The preparation method of above-mentioned Graphene, owing to after dialysis, lyophilization and first thermal reduction, chemistry is gone back
The step such as former, the graphene sheet layer obtained is less, Graphene product i.e. by the less number of plies with benzene ring structure (i.e.
Hexagonal honeycomb structure) the most closelypacked carbon atom stacking composition, the quality of Graphene is higher.Separately
Outward, preparation method provided by the present invention, its raw material is conventional, and cost is relatively low, and required equipment is simply,
Early investment is relatively low, can effectively reduce manufacturing cost.
Present invention also offers a kind of Graphene.
A kind of Graphene, it is obtained by preparation method provided by the present invention.
Above-mentioned Graphene, owing to being obtained by preparation method provided by the present invention, its lamella is less, graphite
The quality of alkene is higher.
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment one
2g graphite (300 mesh) and 2g sodium nitrate are joined in the there-necked flask of dry anhydrous 1000ml,
It is then slowly added into the sulphuric acid of concentration 98wt% of 46ml.There-necked flask is placed on magnetic stirring apparatus addition turn
Son stirring reaction 30min.By 6g KMnO4Join and there-necked flask continues stirring ice bath reaction 2h.So
After there-necked flask is put into 35 DEG C of heating in water bath 1h.The deionized water dropper measuring 92ml is slowly dropped to
In there-necked flask, add in 10min, after adding, be put into 98 DEG C of oil bath pan stirring 30min.Then add
280ml water, adds the H of the 30wt% of 20ml2O2, (40ml's is dense to be eventually adding 400mlHCl solution
Hydrochloric acid, the water of 360ml), it is thus achieved that the liquid of graphene oxide.
Bag filter (model MD44, current-carrying molecular weight: 8000-14000) is placed in boiling water and boils 10 minutes.
The liquid seal of graphene oxide will be obtained in the bag filter boiled, and put the dialysis filling deionized water into
In device, making bag filter between two 260 type platinum electrodes of dialysis apparatus, voltage is set to 25V,
Within one day, change a deionized water, change water continuously two weeks.
After waiting to terminate dialysis, graphene oxide in bag filter is fully washed and is dried.
Take dry graphene oxide 0.1g to join in 500ml deionized water, and ultrasonic agitation, then exist
Take out after stored frozen 24h at-20 DEG C, finally put into and freeze dryer is dried 48h, freeze dryer
Cryogenic temperature is set to-55 DEG C, and vacuum is set to 17Pa.
By the Graphene after lyophilization, argon stove is heated, when in graphite tube in argon stove, temperature reaches
It is passed through argon after 1050 DEG C, and uses CO210MPa is transferred to by pressure regulator；Then the oxygen after lyophilization will be loaded with
The corundum crucible of functionalized graphene is put in graphite tube, heats 30s, has heated and taken out at once, obtained thermal reduction
Product.
Thermal reduction product is joined in 400ml deionized water, ultrasonic 120min.By 20ml weak ammonia
(pH=10) and the hydrazine hydrate of 7ml join ultrasonic after container in, magnetic agitation 4h at 80 DEG C, after
Sucking filtration is also vacuum dried.
Obtain Graphene, be denoted as A1.
Comparative example 1
2g graphite (300 mesh) and 2g sodium nitrate are joined in the there-necked flask of dry anhydrous 1000ml,
It is then slowly added into the sulphuric acid of concentration 98wt% of 46ml.There-necked flask is placed on magnetic stirring apparatus addition turn
Son stirring reaction 30min.By 6g KMnO4Join and there-necked flask continues stirring ice bath reaction 2h.So
After there-necked flask is put into 35 DEG C of heating in water bath 1h.The deionized water dropper measuring 92ml is slowly dropped to
In there-necked flask, add in 10min, after adding, be put into 98 DEG C of oil bath pan stirring 30min.Then add
280ml water, adds the H of the 30wt% of 20ml2O2, (40ml's is dense to be eventually adding 400mlHCl solution
Hydrochloric acid, the water of 360ml), finally wash and be dried.
Take dry graphene oxide 0.1g and join in 400ml deionized water, ultrasonic 120min.By 20ml
The hydrazine hydrate of weak ammonia (pH=10) and 7ml join ultrasonic after container in, magnetic agitation at 80 DEG C
4h, rear sucking filtration is also vacuum dried.
Obtain Graphene, be denoted as B1.
Performance test
SEM tests:
Materials A 1 and B1 is done little multiplying power electron-microscope scanning respectively, and SEM figure is shown in Fig. 1 and Fig. 2 respectively.
Can be seen that from Fig. 1 and Fig. 2, relative material B1, the lamella of the Graphene of materials A 1 substantially to lack very
Many, its quality is higher.
Materials A 1 is done big multiplying power electron-microscope scanning, and SEM figure is shown in Fig. 3-6 respectively.
Can be seen that from Fig. 3 to Fig. 6, the Graphene of materials A 1 possesses that lamella area is big and the characteristic of the low number of plies,
The big explanation of lamella area is the Graphene product that appearance structure is good.It is to say, the Graphene of the present invention its
Quality is more excellent.
Raman spectrum is tested:
Materials A 1 is done Raman spectrum test, and test result is shown in Fig. 7.
From figure 7 it can be seen that materials A 1 has normal D peak and the G being prepared Graphene by oxidation-reduction method
Peak.
Claims (10)
1. the preparation method of a Graphene, it is characterised in that comprise the steps:
Graphene oxide is provided；
Described graphene oxide is dialysed；
Graphene oxide after dialysis is carried out lyophilization；
Graphene oxide after lyophilization is carried out thermal reduction, obtains thermal reduction product；
Described thermal reduction product is carried out electronation, obtains Graphene.
The preparation method of Graphene the most according to claim 1, it is characterised in that described electronation
Using hydrazine hydrate as reducing agent.
The preparation method of Graphene the most according to claim 1, it is characterised in that described thermal reduction
Temperature is 950～1150 DEG C, and the time is 20～30s.
The preparation method of Graphene the most according to claim 3, it is characterised in that described thermal reduction exists
Pressure is to carry out under 8～12MPa.
The preparation method of Graphene the most according to claim 1, it is characterised in that described dialysis is made
The current-carrying molecular weight of dialyzer be 8000～14000.
The preparation method of Graphene the most according to claim 5, it is characterised in that described dialysis it
Before, also include described dialyzer is boiled in boiling water 7～15min.
The preparation method of Graphene the most according to claim 1, it is characterised in that described dialysis be
Deionized water carries out unidirectional current dialysis, and the electrodialytic voltage of direct current is 25V, and the time is for being not less than 30 days and every
It changes deionized water.
The preparation method of Graphene the most according to claim 1, it is characterised in that described lyophilization
Temperature be-50～-70 DEG C, vacuum is 10～30Pa.
The preparation method of Graphene the most according to claim 1, it is characterised in that described graphite oxide
Alkene obtains by improving Hummers method.
10. a Graphene, it is characterised in that the described Graphene preparation by any one of claim 1-9
Method obtains.
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| CN107055523A (en) * | 2016-12-28 | 2017-08-18 | 中国电子科技集团公司第十八研究所 | A kind of method for preparing high stable graphene oxide dispersion |
| CN109037616A (en) * | 2018-07-10 | 2018-12-18 | 桂林理工大学 | Change the method for preparing high performance LiFePO4/three-dimensional graphene composite material by the morphology and size of ferric phosphate |
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| CN103303909A (en) * | 2013-05-30 | 2013-09-18 | 同济大学 | Method for preparing hydrophilic graphene with pH sensitivity |
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Application publication date: 20160928 |