CN107381542A - A kind of preparation facilities of graphene film and preparation method thereof - Google Patents
A kind of preparation facilities of graphene film and preparation method thereof Download PDFInfo
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- CN107381542A CN107381542A CN201710801485.8A CN201710801485A CN107381542A CN 107381542 A CN107381542 A CN 107381542A CN 201710801485 A CN201710801485 A CN 201710801485A CN 107381542 A CN107381542 A CN 107381542A
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- tin liquor
- graphene
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- graphene film
- tin
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Abstract
The present invention relates to a kind of preparation facilities of graphene film, including tin liquor pond（1）, in tin liquor pond built with tin liquor（19）, divider wall is provided with tin liquor pond（2）, the cavity in tin liquor pond is divided into spraying chamber by divider wall（3）And film forming chamber（4）, divider wall side top is provided with upper connected entrance（5）, be provided with lower connected entrance below opposite side（6）, tin liquor pond upside passes through liquid feed device（12）Connect shower nozzle（7）, spraying chamber upside is provided with heater（8）, the upside of film forming chamber is provided with linear electric motors（9）And cooling device（10）.Advantages of the present invention：The present apparatus is effectively utilized low concentration and the small graphene dispersing solution of lamella size, the hot environment of tin liquor makes unnecessary dispersant and high boiling organic solvent thoroughly remove, obtain the graphene film of individual layer or few layer, the ability of the graphene sheet layer of present apparatus aggregation simultaneously is especially strong, and it is simple in construction, it is easy to operate.
Description
Technical field
The present invention relates to technical field of graphene, the preparation facilities of more particularly to a kind of graphene film and its preparation side
Method.
Background technology
The preparation method of graphene mainly has at present：Mechanical stripping method, epitaxial growth method, oxidation-reduction method, chemical gaseous phase
Sedimentation and liquid phase stripping method, liquid phase stripping method therein are by specific solvent or surfactant, with the method for ultrasound
Graphite is peeled off in a solvent, the few single or multiple lift graphene of defect can be obtained.Compared with method above, liquid phase stripping
High in prepare with scale, quality of graphene from method, easy functionalization, raw material are extensive, technique and equipment are simple, the cheap grade side of cost
Face body has unique advantage.
But the graphene dispersing solution prepared with liquid phase stripping method still has several respects when its industrial applications
Problems demand solves, and these problems include：1st, the concentration of graphene dispersing solution is very low；2nd, graphene sheet layer size is too small；3rd, it is more
Remaining dispersant is difficult to remove, high boiling organic solvent is difficult to volatilize；4th, graphite dilute deposit to is prepared into film in substrate
When, excessively slow solvent evaporation rate can cause graphite is dilute to reunite, it is difficult to obtain the graphene film of individual layer or few layer.
The content of the invention
The invention aims to solve the graphene dispersing solution of liquid phase stripping method preparation in background technology in application
The problem of existing, and preparation facilities of a kind of graphene film proposed and preparation method thereof.
To achieve these goals, present invention employs following technical scheme：
A kind of preparation facilities of graphene film, it is characterised in that：Including tin liquor pond, in tin liquor pond built with tin liquor, in tin liquor
Divider wall is provided with pond, the cavity in tin liquor pond is divided into spraying chamber and film forming chamber, set above divider wall side by divider wall
The lower section for having upper connected entrance, opposite side is provided with lower connected entrance, is provided with liquid feed device in the upside in tin liquor pond, liquid feed device is by entering
Liquid pipe connects shower nozzle, and shower nozzle is arranged on the upside of spraying chamber, heater is additionally provided with the upside of spraying chamber, in the upper of film forming chamber
Side is provided with linear electric motors and cooling device.
The preparation facilities can have technical scheme further below on the basis of above-mentioned technical proposal：
Be connected a valve on described at connected entrance and the lower connected entrance.
The training wall of V-type is provided with the spraying intracavitary, the openend of training wall is connected on the divider wall.
Open-mouth mating connection seal closure on the upside of the tin liquor pond, it is provided with the seal closure on the upside of the spraying chamber
Exhaust outlet, exhaust outlet connect emission-control equipment by blast pipe, air admission hole are provided with the seal closure on the upside of the film forming chamber,
Air admission hole connects feeder by air inlet pipe.
The tapping valve for being used for discharging tin liquor is provided with the bottom of the film forming chamber.
A kind of preparation method of graphene film, it is characterised in that comprise the following steps：
Step 1: prepare graphene dispersing solution；
Step 2: graphene dispersing solution is sprayed to the tin liquor surface of melting, the solvent in dispersion liquid is by thermal evaporation volatilization, graphite
Alkene lamella then swims in tin liquor surface in dispersity；
Step 3: the graphene sheet layer of the scattered floating state of driving is concentrated to a regional area on tin liquor surface, formed continuous
The area in flakes of lamella；
Step 4: stopping spraying, the coherent condition in area in flakes is maintained, discharges the tin liquor of 90%-95% below area in flakes；
Step 5: producing tinfoil paper, the temperature in area in flakes is down to normal temperature, remaining tin liquor is frozen into tinfoil paper, while on tinfoil paper
Adhere to a layer graphene film；
Step 6: preparing graphene film, using solvent being dissolved with the tinfoil paper on graphene film, it is thin to obtain graphene
Film.
Following technical scheme can also be up used on the basis of method：
The graphene dispersing solution is prepared using liquid phase stripping method.
The advantage of the invention is that：The present apparatus is effectively utilized low concentration and the small graphene dispersing solution of lamella size,
The hot environment of tin liquor makes unnecessary dispersant and high boiling organic solvent thoroughly remove, due to solvent at high temperature rapid
Volatilization, and suction-operated of the tin liquor to graphene sheet layer, make the dilute lamella of graphite be difficult to reunite, and obtain individual layer or lack layer
Graphene film, while the ability of present apparatus aggregation graphene sheet layer is especially strong and simple in construction, it is easy to operate.
Brief description of the drawings
Fig. 1 is the basic structure schematic diagram of the present invention（Fig. 2 A-A sectional views）；
Fig. 2 is Fig. 1 B-B sectional views；
Fig. 3 is Fig. 2 side view.
Embodiment
In order that the present invention is more clearly understood, the present apparatus is described in detail below in conjunction with accompanying drawing, tool described herein
Body embodiment only to explain the present invention, is not intended to limit the present invention.
As shown in Figure 1, Figure 2 and Figure 3, a kind of preparation facilities of graphene film provided by the invention includes tin liquor pond 1, tin
Liquid pool 1 is prior art, is provided with opening in the upside in tin liquor pond 1, the open-mouth mating connection seal closure in the upside of tin liquor pond 1
14。
In tin liquor pond 1 built with tin liquor 19, divider wall 2, cavity point of the divider wall 2 tin liquor pond 1 are provided with tin liquor pond 1
Spraying chamber 3 and film forming chamber 4 are cut into, the training wall 11 of V-type is provided with spraying chamber 3, the openend of training wall 11 is connected to isolation
On wall 2, divider wall 2 forms the wall that cross section is triangular structure with training wall 11, is provided with the bottom of film forming chamber 4 and is used to arrange
Put the tapping valve 13 of tin liquor.
Lower connected entrance 6 is provided with lower section of the top of the side of divider wall 2 provided with upper connected entrance 5, opposite side, in upper connected entrance
5 and lower connected entrance 6 at be connected a valve, two valves are not drawn into figure, and its structure is prior art, close
The outside of sealing cover 14 is provided with liquid feed device 12, and liquid feed device 12 is also prior art, and liquid feed device 12 is connected by feed tube 20 to be sprayed
First 7, shower nozzle 7 is arranged on the upside of spraying chamber 3 inside seal closure 14, and heater 8 is additionally provided with the upside of spraying chamber 3, into
The upside of membrane cavity 4 is provided with linear electric motors 9 and cooling device 10, and cooling device 10 is prior art.
The linear electric motors 9 are a kind of equipment for directly converting electrical energy into mechanical energy, when linear electric motors three-phase windings lead to
When entering alternating current, travelling-magnetic-field will be produced, the conductor in travelling-magnetic-field induces electric current because of cutting magnetic line, electric current
Electromagnetic force is just produced with magnetic field interaction, this electromagnetic force promotes tin liquor 19 described in conducting liquid along the arrow in Fig. 1 and Fig. 2
Flowing.
Linear electric motors 9 do not contact with tin liquor 19, guide the tin liquor of spraying intracavitary fixed by upper connected entrance 5 using linear electric motors
To flowing into film forming chamber, the graphene sheet layer of floating is stayed in film forming chamber using divider wall, returned tin liquor using lower connected entrance 6
Spraying intracavitary is flowed into, water conservancy diversion is carried out to tin liquor using training wall.With the progress of operation, the graphene on tin liquor surface in film forming chamber
Lamella is on the increase, and under the promotion of tin liquor mobilization force, these lamellas contact with each other, head and the tail connect, and form continuous lamella area
Domain.
Exhaust outlet 16 is provided with the seal closure 14, exhaust outlet 16 connects emission-control equipment 18 by blast pipe 21,
Emission-control equipment 18 is prior art, is provided with air admission hole 15 on the seal closure 14 of the upside of film forming chamber 4, air admission hole 15 is logical
Cross air inlet pipe 22 and connect feeder 17.
In above-mentioned specific embodiment operating process, liquid feed device 12 is that shower nozzle 7 provides raw material liq, and feeder 17 carries
The gas with protection and restoring function supplied is continuously fed to seal closure 14 by air admission hole 15, and emission-control equipment 18 passes through row
Gas port 16 continues waste gas caused by solvent volatilization etc. discharging seal closure 14, and heater 8 is used to keep tin liquor temperature.
The graphene film uses following preparation method on the basis of said apparatus, and concrete operation step is：
Step 1: preparing graphene dispersing solution using existing liquid phase stripping method, the graphene dispersing solution prepared passes through shower nozzle 7
Spray to the surface of tin liquor 19 that melts in spraying chamber 3, the solvent in dispersion liquid is by thermal evaporation volatilization, and graphene sheet layer is then in scattered
State swims in tin liquor surface.
Step 2: starting linear electric motors 9, the tin liquor 19 on upper strata flows into film forming chamber by upper connected entrance 5 in guiding spraying chamber 3
4, the graphene film for swimming in the surface of tin liquor 19 is isolated wall 2 and stopped, be trapped in film forming chamber 4, lower floor's tin liquor 19 is then from isolation
2 times subordinate's connected entrances 6 of wall are flowed back in spraying chamber 3 so that tin liquor 19 circulates.
Step 3: leaving the speed of spraying chamber 3 according to the graphene sheet layer of floating, shower nozzle 7 is kept to be in accomplished continuously or intermittently
State, with the progress of operation, the graphene sheet layer on the surface of tin liquor 19 is constantly assembled in film forming chamber 4, these lamellas contact with each other,
Head and the tail connect, and form the area in flakes of continuous lamella.
Step 4: after area is full of the surface of film forming chamber 4 in flakes, stop spraying, connected by closing upper connected entrance 5 with
The valve of mouth 6, the tin liquor 19 for spraying chamber 3 and film forming chamber 4 is isolated, open the tapping valve 13 of the bottom of film forming chamber 4, discharge tin liquor 19
To closing tapping valve 13 when only retaining a thin layer tin liquor.
Step 5: starting the cooling device 10 of film forming chamber 4, the temperature in the film forming chamber 4 is set to be reduced to normal temperature, then thin layer tin
Liquid is frozen into tinfoil paper, adheres to a layer graphene film thereon.
Step 6: taking out above-mentioned tinfoil paper, tinfoil paper is dissolved with suitable solvent, obtains the graphene of large area continuous uniform
Film.
Claims (7)
- A kind of 1. preparation facilities of graphene film, it is characterised in that：Including tin liquor pond（1）, in tin liquor pond（1）Built with tin liquor （19）, in tin liquor pond（1）It is interior to be provided with divider wall（2）, divider wall（2）Tin liquor pond（1）Cavity be divided into spraying chamber（3）With into Membrane cavity（4）, in divider wall（2）The top of side is provided with upper connected entrance（5）, opposite side lower section be provided with lower connected entrance（6）, in tin Liquid pool（1）Upside be provided with liquid feed device（12）, liquid feed device（12）Pass through feed tube（20）Connect shower nozzle（7）, shower nozzle（7）If Put in spraying chamber（3）Upside, spraying chamber（3）Upside be additionally provided with heater（8）, in film forming chamber（4）Upside be provided with Linear electric motors（9）And cooling device（10）.
- A kind of 2. preparation facilities of graphene film according to claim 1, it is characterised in that：The connected entrance on described （5）With the lower connected entrance（6）Place's one valve of mating connection.
- A kind of 3. preparation facilities of graphene film according to claim 1 and preparation method thereof, it is characterised in that：Institute State spraying chamber（3）The interior training wall provided with V-type（11）, training wall（11）Openend be connected to the divider wall（2）On.
- A kind of 4. preparation facilities of graphene film according to claim 1, it is characterised in that：In the tin liquor pond（1） The open-mouth mating connection seal closure of upside（14）, in the spraying chamber（3）The seal closure of upside（14）It is provided with exhaust outlet （16）, exhaust outlet（16）Pass through blast pipe（21）Connect emission-control equipment（18）, in the film forming chamber（4）The seal closure of upside （14）It is provided with air admission hole（15）, air admission hole（15）Pass through air inlet pipe（22）Connect feeder（17）.
- A kind of 5. preparation facilities of graphene film according to claim 1, it is characterised in that：In the film forming chamber（4） Bottom be provided with and be used to discharge the tapping valve of tin liquor（13）.
- 6. a kind of preparation method of graphene film, it is characterised in that comprise the following steps：Step 1: prepare graphene dispersing solution；Step 2: graphene dispersing solution is sprayed to the tin liquor of melting（19）Surface, solvent in dispersion liquid by thermal evaporation volatilization, Graphene sheet layer then swims in tin liquor surface in dispersity；Step 3: the graphene sheet layer of the scattered floating state of driving is concentrated to a regional area on tin liquor surface, formed continuous The area in flakes of lamella；Step 4: stopping spraying, the coherent condition in area in flakes is maintained, discharges the tin liquor 19 of 90%-95% below area in flakes；Step 5: producing tinfoil paper, the temperature in area in flakes is down to normal temperature, remaining tin liquor（19）Tinfoil paper is frozen into, while in tin Adhere to a layer graphene film on paper tinsel；Step 6: preparing graphene film, using solvent being dissolved with the tinfoil paper on graphene film, it is thin to obtain graphene Film.
- 7. preparation method according to claim 6, it is characterised in that：The graphene dispersing solution peels off legal system using liquid phase It is standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710801485.8A CN107381542A (en) | 2017-09-07 | 2017-09-07 | A kind of preparation facilities of graphene film and preparation method thereof |
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| CN201710801485.8A CN107381542A (en) | 2017-09-07 | 2017-09-07 | A kind of preparation facilities of graphene film and preparation method thereof |
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| CN102674333A (en) * | 2012-05-23 | 2012-09-19 | 西安电子科技大学 | Method for preparing structured graphene based on reaction of Cl2 and Ni film annealing |
| CN102942178A (en) * | 2012-11-22 | 2013-02-27 | 武汉大学 | Compound base of precious metal nanometer array and single layer graphene and preparation method thereof |
| CN103043654A (en) * | 2011-10-12 | 2013-04-17 | 国家纳米科学中心 | Film containing graphene and/or graphene oxide, and preparation method thereof |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN105965025A (en) * | 2016-07-13 | 2016-09-28 | 江苏省特种设备安全监督检验研究院 | Method and device for producing high-strength and high-conductivity graphene copper-based powder material |
| CN106629675A (en) * | 2016-09-28 | 2017-05-10 | 上海理工大学 | Preparation method of high-heat-conduction flexible graphene film |
| CN107032328A (en) * | 2016-02-02 | 2017-08-11 | 中国科学院理化技术研究所 | A kind of preparation method of self-supporting oxidation graphene film |
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2017
- 2017-09-07 CN CN201710801485.8A patent/CN107381542A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043654A (en) * | 2011-10-12 | 2013-04-17 | 国家纳米科学中心 | Film containing graphene and/or graphene oxide, and preparation method thereof |
| CN102674333A (en) * | 2012-05-23 | 2012-09-19 | 西安电子科技大学 | Method for preparing structured graphene based on reaction of Cl2 and Ni film annealing |
| CN102942178A (en) * | 2012-11-22 | 2013-02-27 | 武汉大学 | Compound base of precious metal nanometer array and single layer graphene and preparation method thereof |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN107032328A (en) * | 2016-02-02 | 2017-08-11 | 中国科学院理化技术研究所 | A kind of preparation method of self-supporting oxidation graphene film |
| CN105965025A (en) * | 2016-07-13 | 2016-09-28 | 江苏省特种设备安全监督检验研究院 | Method and device for producing high-strength and high-conductivity graphene copper-based powder material |
| CN106629675A (en) * | 2016-09-28 | 2017-05-10 | 上海理工大学 | Preparation method of high-heat-conduction flexible graphene film |
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Application publication date: 20171124 |