CN107601479A - Graphene prepared by the preparation method and this method of a kind of graphene - Google Patents
Graphene prepared by the preparation method and this method of a kind of graphene Download PDFInfo
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- CN107601479A CN107601479A CN201710967829.2A CN201710967829A CN107601479A CN 107601479 A CN107601479 A CN 107601479A CN 201710967829 A CN201710967829 A CN 201710967829A CN 107601479 A CN107601479 A CN 107601479A
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- ethyl alcohol
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Abstract
The present invention provides graphene prepared by a kind of preparation method of graphene and this method, belongs to technical field of graphene.The preparation method of graphene, absolute ethyl alcohol, dispersant and graphite powder are sequentially added into progress vacuum machine in container and disperseed.Wherein：The mass ratio of absolute ethyl alcohol, dispersant and graphite powder is followed successively by (5 50)：1：(2.5‑10).The thickness of graphene prepared by this preparation method is controllable, and oxygen content is low, and conductance is high, and preparation method is simple, is advantageous to produce on a large scale.
Description
Technical field
The present invention relates to technical field of graphene, preparation method and party's legal system in particular to a kind of graphene
Standby graphene.
Background technology
Graphene is that the two dimensional crystal material of monoatomic layer is also structure carbon material the simplest.Common graphite material
It is considered as being formed by graphene stacked in multi-layers, therefore graphene is also considered " mono-layer graphite ".It is described as " 21 century mystery material
The graphene of material " is that the world being currently known is most thin, most hard, electric conductivity is best at room temperature and possesses receiving for powerful flexibility
Rice material：It can separate 3,000,000 layer graphenes with the thickness of thin to only one carbon atom in the graphite of 1 millimeters thick；It
Very hard, its intensity is more taller 200MPa than steel；At room temperature, the minimum metal of resistivity is silver, and the resistivity ratio of graphene
Silver is also small；Its transparent and air-locked characteristic makes application of the graphene future in numerous areas such as touch-screen, sensor, batteries
Full of the imagination.At present, the market price of graphene raw material graphite is about 3000 yuan/ton, and after being refined into graphene, graphene
Market price be up to 1,000,000/ton.
The thickness of the graphene of prior art is uncontrollable, and oxygen content is high, and preparation method is complicated, is unfavorable for mass producing.
The content of the invention
It is an object of the invention to provide a kind of preparation method of graphene, method is simple, beneficial to operation, the graphite of preparation
Alkene thickness is controllable, and oxygen content is low, and conductance is high.
The graphene prepared another object of the present invention is to provide a kind of above method, thickness is controllable, and oxygen content is low, leads
Electric rate is high.
The present invention is realized using following technical scheme：
A kind of preparation method of graphene, absolute ethyl alcohol, dispersant and graphite powder is sequentially added vacuum is carried out in container
Mechanical dispersion.
Wherein：The mass ratio of absolute ethyl alcohol, dispersant and graphite powder is followed successively by (5-50)：1：(2.5-10).
A kind of graphene, it is prepared by the preparation method of above-mentioned graphene.
The beneficial effect of preparation method for the graphene that presently preferred embodiments of the present invention provides is：Absolute ethyl alcohol is first added,
Adding dispersant, absolute ethyl alcohol makes dispersant be dissolved in absolute ethyl alcohol as solvent, when graphite powder is added, graphite
The surface attachment of powder has dispersant, graphite powder is dispersed in anhydrous ethanol solvent, then carries out vacuum machine and disperse, vacuum
During mechanical dispersion, dispersant molecule is embedded into the Rotating fields gap of graphite, the synergy disperseed with vacuum machine,
The charge stripping efficiency of graphite flake layer can be improved, dispersion effect is good, obtains graphene.Further, since it is the vacuum condition in hypoxemia
Lower to carry out mechanical fraction, gained graphene oxygen content is low, conducts electricity very well.And because absolute ethyl alcohol is both as solvent as scattered
Thermit powder, it can make it that caused heat is effectively distributed during high speed spheroidal graphite, so as to reduce the thermal deformation of graphene.Together
When, the effect of dispersant avoids graphene from assembling, and obtains the fabulous graphene suspension of high uniformity, dispersiveness, puts
Postponing to be layered, and be advantageous to its practical application and compound other materials.
Graphene provided by the invention has the beneficial effect that：The thickness of graphene prepared by the above method is controllable, oxygen content
Low, conductance is high.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below by embodiment it is required use it is attached
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, therefore be not construed as pair
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings and fall within protection scope of the present invention.
Fig. 1 is the scanning electron microscope analysis picture for the graphene that the embodiment of the present invention 1 provides；
Fig. 2 is the AFM Analysis picture for the graphene that the embodiment of the present invention 1 provides；
Fig. 3 is the XPS analysis picture for the graphene that the embodiment of the present invention 1 provides.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, it is the conventional production that can be obtained by commercially available purchase
Product.
The preparation method of graphene and the graphene of this method preparation of the embodiment of the present invention are specifically described below.
The preparation method of graphene comprises the following steps：
The first step：Absolute ethyl alcohol, dispersant and graphite powder are sequentially added into progress vacuum machine in container to disperse.First add
Absolute ethyl alcohol, adds dispersant, and absolute ethyl alcohol makes dispersant be dissolved in absolute ethyl alcohol, adding graphite powder as solvent
When, the surface attachment of graphite powder has dispersant, graphite powder is dispersed in anhydrous ethanol solvent, then carries out vacuum machine
Scattered, during vacuum machine is scattered, dispersant molecule is embedded into the Rotating fields gap of graphite, disperses with vacuum machine
Synergy, can improve the charge stripping efficiency of graphite flake layer, dispersion effect is good, obtains graphene.Additionally, due to being in hypoxemia
Mechanical fraction is carried out under vacuum condition, gained graphene oxygen content is low, conducts electricity very well.And because absolute ethyl alcohol is both used as solvent
Coolant is used as again, can make it that caused heat is effectively distributed during high speed spheroidal graphite, so as to reduce graphene
Thermal deformation.Meanwhile the effect of dispersant avoids graphene from assembling, the fabulous graphene of high uniformity, dispersiveness is obtained
It suspension, will not be layered after placement, be advantageous to its practical application and compound other materials.
The mass ratio of absolute ethyl alcohol, dispersant and graphite powder is followed successively by (5-50)：1：(2.5-10).Dispersant is to graphite powder
Peeling effect it is preferable, meanwhile, the amount of dispersant will not be excessive, facilitates dispersant to be separated with the graphene prepared, obtains
To pure graphene.
Preferably, the particle diameter of graphite powder is 100 mesh to 500 mesh, and the graphite powder cost of the particle diameter is low, reduces the system of graphene
Standby cost.
In the present invention, dispersant is selected from sodium taurocholate or 1-METHYLPYRROLIDONE.
Wherein：Sodium taurocholate is ionic surfactant, is a kind of parents' molecule, can both have been adsorbed in graphite surface, together
When also be soluble in absolute ethyl alcohol, play a part of preventing graphene from reuniting；And sodium taurocholate without fixation critical micelle concentration,
Sufficient effect can be played during preparing graphene, improves the preparation efficiency of graphene.Sodium taurocholate is except playing surface
Beyond the function of activating agent, because it uniformly exists in solution in mechanical dispersion, cholic acid sodium molecule can be embedded into graphite
Lamellar structure gap in, with the stripping to graphite flake layer can be greatly improved under the synergy of the mechanical force of mechanical dispersion
Efficiency, so as to obtain a kind of homogeneous few layer graphene structure of property, the efficiency of mechanical dispersion is also improved, obtains height
The graphene suspension that degree is uniform, dispersiveness is fabulous.
1-METHYLPYRROLIDONE is amine compound, and it is a kind of organic compound, is decomposed during mechanical dispersion
Into small-molecule substance, it can be more prone to be embedded into the gap of graphitic molecules, so as to accelerate the stripping of graphite flake layer, obtain thickness
Spend controllable graphene.
Preferably, mechanical dispersion comprises the following steps：
1st, absolute ethyl alcohol, dispersant and graphite powder are sequentially added in agitator tank and stirred, further made absolute ethyl alcohol, disperse
Agent and graphite powder are well mixed, and dispersant is got more preferable effect in prepared by follow-up graphene.
Specifically, 5min-10min is stirred under conditions of room temperature (20 DEG C -30 DEG C), makes three kinds of materials can be good at mixing
Close.
2nd, the absolute ethyl alcohol after stirring, dispersant and graphite powder are ultrasonically treated using Ultrasound Instrument, are ultrasonically treated
The motion of molecules in solution can be accelerated, make its mixing more uniform, simultaneously as the effect of ultrasound, the temperature rise of solution,
Make molecular motion more obvious, be advantageous to the stripping of graphite flake layer.
Specifically, supersound process 5min-10min is carried out under conditions of ultrasonic power is 200w-500w.With being stirred
Compare, supersound process can make to be well mixed between various material molecules and molecule, send out the effect of dispersant in subsequent process
Maximum is waved, the preparation efficiency of graphene is multiplied.
3rd, the mixed solution after supersound process is poured into progress vacuum ball milling in ball grinder, passes through the shearing of vacuum ball milling
Power, the dispersant for making to be well mixed with graphite powder are constantly embedded in the Rotating fields gap of graphite, graphite flake layer are peeled off, make
For going out, thickness is controllable, and oxygen content is low, the high graphene of conductance.
Specifically, ball milling carries out 7h- under conditions of vacuum is 10Pa-50Pa, rotating speed is 300r/min-500r/min
20h.The thickness that prolonged ball milling makes obtained graphene is more uniform, and the purity and yield of graphene are all higher, while
Operated under vacuum wet method, ensure that low oxygen content, high conductivity and the low deformation extent of graphene.
In the present invention, in order that the thickness of graphene is smaller, the oxygen content of graphene is lower, and conductance is higher, in addition to
Second step：Nanosizing processing is carried out to the solution after ball milling.
Nanosizing processing uses high pressure homogenizer, ultrasonic emulsification machine or high pressure cell cracker.Its run at high speed to containing
The solution for having graphene applies very big shearing force, and graphite flake layer is peeled off, and the thickness of obtained graphene is smaller, uses
Value is higher.
Preferably, the time of nanosizing processing is 10min-20min.
3rd step：It is dried, obtains pure in freeze drier using washes of absolute alcohol graphene solution, then by it
Net graphene product.
Graphene made from the preparation method of the above-mentioned graphene of the present invention, its thickness are 3-4nm, and oxygen content is 4at.% left
The right side, the thickness of graphene is controllable, and oxygen content is low, and conductance is high, is advantageous to practical application and compound other materials.
Embodiment 1
5g absolute ethyl alcohols, 1g dispersants and 2.5g graphite powders are sequentially added into progress vacuum machine in container to disperse to obtain stone
Black alkene.
The graphene solution that embodiment 1 obtains is cleaned using absolute ethyl alcohol, then it is dried in freeze drier, is obtained
To the graphene of clean dry.Dry graphene is used into scanning electron microscope analysis, obtains Fig. 1, from Fig. 1 can clearly from
To the pattern of graphene, the thickness of graphene is 3-4nm, its thickness uniform, controllable.Dry graphene is shown using atomic force
Micro mirror is analyzed, and obtains Fig. 2, as can be seen from Figure 2：The number of plies of graphene is 4 layers.Dry graphene is used into X ray photoelectricity
Sub- energy spectrometer analysis, Fig. 3 is obtained, as can be seen from Figure 3：The oxygen content of graphene is relatively low, makes the conductance of graphene high, expands
The use range of graphene.
Embodiment 2
50g absolute ethyl alcohols, 1g sodium taurocholates and 10g graphite powders are sequentially added 5min is stirred in agitator tank, then in ultrasonic work(
Rate is to be ultrasonically treated 10min in 200w Ultrasound Instrument, after pour into the ball grinder that vacuum is 50Pa, rotating speed is 300r/min it is true
Empty ball milling 20h obtains graphene.
Embodiment 3
10g absolute ethyl alcohols, 1g sodium taurocholates and 5g graphite powders are sequentially added 10min is stirred in agitator tank, then in ultrasonic work(
Rate is to be ultrasonically treated 5min in 500w Ultrasound Instrument, after pour into the ball grinder that vacuum is 10Pa, rotating speed is 500r/min it is true
Empty ball milling 7h, then carry out nanosizing and handle to obtain graphene.
Embodiment 4
40g absolute ethyl alcohols, 1g sodium taurocholates and 8g graphite powders are sequentially added 8min is stirred in agitator tank, then in ultrasonic power
To be ultrasonically treated 7min in 400w Ultrasound Instrument, after pour into vacuum in the ball grinder that vacuum is 20Pa, rotating speed is 400r/min
Ball milling 10h, reuse high pressure homogenizer progress nanosizing processing 10min and obtain graphene.
Embodiment 5
40g absolute ethyl alcohols, 1g sodium taurocholates and 8g graphite powders are sequentially added 8min is stirred in agitator tank, then in ultrasonic power
To be ultrasonically treated 7min in 400w Ultrasound Instrument, after pour into vacuum in the ball grinder that vacuum is 40Pa, rotating speed is 400r/min
Ball milling 10h, reuse ultrasonic emulsification machine progress nanosizing processing 20min and obtain graphene.
Embodiment 6
40g absolute ethyl alcohols, 1g sodium taurocholates and 8g graphite powders are sequentially added 8min is stirred in agitator tank, then in ultrasonic power
To be ultrasonically treated 7min in 400w Ultrasound Instrument, after pour into vacuum in the ball grinder that vacuum is 50Pa, rotating speed is 400r/min
Ball milling 10h, reuse high pressure cell cracker progress nanosizing processing 15min and obtain graphene.
Comparative example 1
40g absolute ethyl alcohols and 8g graphite powders are sequentially added into progress mechanical dispersion in container and obtain graphene.
The obtained graphene solution of embodiment 1-6 and comparative example 1 is cleaned using absolute ethyl alcohol, then it is being freeze-dried
Dried in machine, obtain the graphene of clean dry.
Embodiment 1-6 and the graphene of comparative example 1 are scanned into 3 pictures using ESEM respectively, determine its thickness；Will
Embodiment 1-6 and the graphene of comparative example 1 obtain its oxygen content, analysis such as table 1 using x-ray photoelectron spectroscopy respectively.
Table 1
From table 1 it follows that compared with the thickness of the graphene prepared with comparative example 1, the graphite of embodiment 1-6 preparations
The thickness ratio of alkene is more uniform, meanwhile, thickness is controllable, can be advantageous to graphene according to the thickness of different demand modeling graphenes
Practice, meanwhile, it is capable to produce relatively thin graphene, utilization is more extensive.From table 1 it follows that with comparative example 1
The oxygen content of the graphene of preparation compares, embodiment 1-6 prepare graphene oxygen content it is relatively low, so as to get graphene
Conductance it is higher, beneficial to the application of graphene.
Embodiments described above is part of the embodiment of the present invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of preparation method of graphene, it is characterised in that sequentially add absolute ethyl alcohol, dispersant and graphite powder in container
Vacuum machine is carried out to disperse；
Wherein：The mass ratio of the absolute ethyl alcohol, the dispersant and the graphite powder is followed successively by (5-50)：1：(2.5-10).
2. preparation method according to claim 1, it is characterised in that the dispersant is sodium taurocholate or N- crassitudes
Ketone.
3. preparation method according to claim 1, it is characterised in that by the absolute ethyl alcohol, the dispersant and described
Graphite powder is sequentially added in agitator tank and stirred, then pours into progress vacuum ball milling in ball grinder.
4. preparation method according to claim 3, it is characterised in that by the absolute ethyl alcohol, the dispersant and described
Graphite powder sequentially add in agitator tank stir after, poured into after being ultrasonically treated in Ultrasound Instrument and vacuum sphere carried out in ball grinder
Mill obtains.
5. preparation method according to claim 4, it is characterised in that the supersound process is 200w- in ultrasonic power
5min-10min is carried out under conditions of 500w.
6. preparation method according to claim 4, it is characterised in that the ball milling is 10Pa-50Pa, rotating speed in vacuum
To carry out 7h-20h under conditions of 300r/min-500r/min.
7. preparation method according to claim 4, it is characterised in that after the vacuum ball milling, in addition to carry out nanometer
The step of changing processing.
8. preparation method according to claim 7, it is characterised in that the nanosizing processing uses high pressure homogenizer, surpassed
Sound wave mulser or high pressure cell cracker.
9. preparation method according to claim 7, it is characterised in that the time of the nanosizing processing is 10min-
20min。
10. a kind of graphene, it is characterised in that as the preparation method preparation of the graphene described in claim any one of 1-9
Into.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115259145A (en) * | 2022-07-29 | 2022-11-01 | 武汉汉烯科技有限公司 | Preparation method of high-conductivity macroscopic graphene assembly film close to lower limit of Poisson ratio |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104176727A (en) * | 2013-05-28 | 2014-12-03 | 安炬科技股份有限公司 | Graphene suspended solution and making method thereof |
| CN105129776A (en) * | 2015-07-14 | 2015-12-09 | 合肥工业大学 | Few-layer graphene and preparation method thereof |
| CN105849040A (en) * | 2013-12-26 | 2016-08-10 | 株式会社Lg化学 | Production method for graphene |
| CN105873858A (en) * | 2013-12-26 | 2016-08-17 | 株式会社Lg化学 | Graphene production method, and graphene dispersion composition |
| KR20170015742A (en) * | 2015-07-31 | 2017-02-09 | 가천대학교 산학협력단 | Method of manufacturing non-oxidized graphene using shear flow exfoliation and electrochemical pretreatment and apparatus for manufacturing the same |
-
2017
- 2017-10-16 CN CN201710967829.2A patent/CN107601479A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104176727A (en) * | 2013-05-28 | 2014-12-03 | 安炬科技股份有限公司 | Graphene suspended solution and making method thereof |
| CN105849040A (en) * | 2013-12-26 | 2016-08-10 | 株式会社Lg化学 | Production method for graphene |
| CN105873858A (en) * | 2013-12-26 | 2016-08-17 | 株式会社Lg化学 | Graphene production method, and graphene dispersion composition |
| CN105129776A (en) * | 2015-07-14 | 2015-12-09 | 合肥工业大学 | Few-layer graphene and preparation method thereof |
| KR20170015742A (en) * | 2015-07-31 | 2017-02-09 | 가천대학교 산학협력단 | Method of manufacturing non-oxidized graphene using shear flow exfoliation and electrochemical pretreatment and apparatus for manufacturing the same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115259145A (en) * | 2022-07-29 | 2022-11-01 | 武汉汉烯科技有限公司 | Preparation method of high-conductivity macroscopic graphene assembly film close to lower limit of Poisson ratio |
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