TW201527600A - Apparatus for graphene formation - Google Patents

Abstract

An apparatus for graphene formation is provided. The apparatus includes an electrolytic chamber, at least one first electrode, at least one second electrode, a holder, a graphene formatting material and a porous packing. The electrolytic cell has electrolyte solution. The first electrode is disposed corresponding to the second electrode, and the first and second electrodes are clamped by the holder. The graphene formatting material is disposed on the second electrode, and the porous packing is sandwiched by the first and second electrodes.

Description

Graphene generating device

The invention is a generating device, in particular a graphene generating device.

Graphene is a single layer of atomic carbon material. Each carbon atom is sp ² mixed with adjacent three atoms and forms a honeycomb two-dimensional structure. Moreover, graphene is more famous for its good carrier mobility. Because of its excellent electrical properties, chemical stability, good thermal conductivity and high transmittance, graphene has been widely used. Popular materials in the fields of semiconductors, touch panels or solar cells.

Generally, the formation method of graphene includes mechanical exfoliation, epitaxial growth, chemical vapor deposition (CVD), and chemical exfoliation. Among them, the mechanical exfoliation method and the epitaxial growth method can produce graphene with better quality, but neither method can synthesize graphene in a large amount.

Moreover, if chemical vapor deposition is used, the operating temperature is near a thousand degrees of high temperature and an expensive metal substrate, and the preparation process takes several hours to complete. The shortcomings of these methods limit the production and subsequent application of graphene. The chemical stripping method produces graphene by redoxing the graphite under strong acid and strong oxidation conditions. Although this method is suitable for mass production, the surface structure and size of the graphene produced are less than ideal.

In addition to the above-described production method, graphene can also be produced by an electrochemical stripping method. Its main principle of action is that the interaction between the electrolyte and the graphite surface causes the surface of the graphite material of the anode to be oxidized and stripped. Although the manner of electrochemical stripping is conventionally controlled, it is impossible to control the extent to which the graphite raw material is peeled off from the electrode (may not be completely peeled off), and the space in which the electrolytic cell cannot be efficiently used. However, compared with the other generation methods described above, the electrochemical stripping method can rapidly and economically produce graphene at room temperature, in other words, if the chemical stripping method can be improved, stone The production of ocene will enable the electrochemical stripping method to be an economical and large-scale production method of graphene.

Therefore, how to provide a graphene generating device capable of producing at a normal temperature, low in cost, improving efficiency, and improving overall production quality has become one of the important problems to be solved in the field.

In view of the above problems, an object of the present invention is to provide a graphene generating apparatus which can improve graphene production, production efficiency, and mass production.

To achieve the above object, according to the present invention, there is provided a graphene generating apparatus comprising an electrolytic cell, a jig, at least a first electrode, at least a second electrode, a graphene material, and a porous filler.

The electrolytic cell is filled with the electrolyte, and at least one second electrode is disposed opposite to the first electrode. And the clamp sandwiches the first electrode and the second electrode. The graphene material may be disposed on the second electrode. The porous filler may be disposed between the first electrode and the second electrode.

In an embodiment, the power supply is further connected to the first electrode and the second electrode, respectively, and the first electrode and the second electrode generate a potential difference.

In an embodiment, the first electrode and the second electrode have a potential difference and the potential difference is between 5 volts and 100 volts.

In an embodiment, the potential difference may be between 10 volts and 50 volts.

In one embodiment, a screen is further included between the porous filler and the graphene material.

In an embodiment, the porous filler has a pore size between 5 μm and 1 mm.

In one embodiment, the porous filler material is a porous ceramic plate, a sponge, a foamed plastic, a plastic mesh, a zeolite, a quartz sponge, or a combination thereof.

In an embodiment, the first electrode and the second electrode are made of a graphite material or a metal.

In an embodiment, a liquid inlet unit and an exhaust unit are further included.

According to the above, the present invention can be interposed between the first electrode and the second electrode. The pore filler and the porous filler material allow the electrolyte to react uniformly with the graphene material on the electrode. Therefore, the present invention can achieve the object of providing a graphene generating device which can be produced at normal temperature, has low cost, improves efficiency, and improves overall production quality.

1‧‧‧graphene generating device

10, 10a‧‧‧ Electrolyzer

11, 11a‧‧‧ first electrode

12, 12a‧‧‧ second electrode

13, 13a‧‧‧Graphene materials

14, 14a‧‧‧ Porous filler

15‧‧‧Power supply

16, 16a‧‧‧ Inlet unit

17a‧‧‧Filter

18, 18a‧‧‧ fixture

S‧‧‧ electrolyte

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a perspective view showing a first embodiment of a graphene producing apparatus of the present invention.

Figure 2 is a side elevational view of the embodiment of Figure 1.

Figure 3 is a further graph of the production-through bar graph of the graphene generating apparatus of the present invention and a conventional electrochemical stripping process.

4 is a thickness distribution-proportional bar graph of a graphene generating apparatus and a conventional electrochemical stripping process of the present invention.

Figure 5 is a side elevational view of a second embodiment of a graphene generating apparatus of the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a graphene generating apparatus according to a preferred embodiment of the present invention will be described with reference to the accompanying drawings, wherein the same elements will be described with the same reference numerals.

Please refer to FIG. 1 to FIG. 4, which is a perspective view of a first embodiment of a graphene generating device of the present invention. Figure 2 is a side elevational view of the embodiment of Figure 1. Fig. 3 is a graph showing the yield-bar graph of the graphene generating apparatus of the present invention and a conventional electrochemical stripping process. 4 is a thickness distribution-proportional bar graph of a graphene generating apparatus and a conventional electrochemical stripping process of the present invention.

The graphene generating apparatus 1 of the first embodiment of the present invention includes an electrolytic cell 10, at least a first electrode 11, at least a second electrode 12, a graphene material 13, a porous filler 14, and a jig 18.

The electrolytic cell 10 of the present embodiment has a housing tank to fill the electrolyte S. The electrolytic solution S of the present embodiment may be a graphene solution.

Referring to FIG. 1 and FIG. 2 , at least one second electrode 12 and the first electrode 11 are disposed opposite to each other, and the first electrode 11 and the second electrode 12 can form an electrode module. In addition, the first electrode 11 of the embodiment is an inert electrode made of a graphite material or a metal. Real The second electrode 12 of the embodiment may also be made of a graphite material or a metal. The graphite material or the metal material herein may be made of natural graphite, artificial graphite, copper, stainless steel, platinum, etc., but not These materials are limited.

Further, the graphene material 13 of the present embodiment may be disposed on the second electrode 12. The manner in which the graphene material 13 is disposed may be partially or completely covered by the second electrode 12. Here, the graphene material 13 may be any carbon material having a graphitized arrangement such as natural graphite or artificial graphite.

The porous filler 14 may be disposed between the first electrode 11 and the second electrode 12. In detail, the porous filler 14 can be disposed between the graphene material 13 and the second electrode 12, so that the porous filler 14 provided in the embodiment can avoid the second electrode 12 and the graphene material. 13 contact caused a short circuit problem. Further, the distance between the first electrode 11 and the second electrode 12 (the separation distance is the thickness of the porous filler 14) can be adjusted by different porous fillers 14 to adjust the overall reaction rate. In short, with this configuration of the embodiment, a plurality of electrode modules can be stacked more efficiently in the electrolytic cell 10, and the overall yield can be effectively improved.

Further, the pores on the electrolyte solution S are uniformly guided to the surfaces of the first electrode 11 and the second electrode 12, and an electrochemical reaction is generated. Finally, the gas generated in the electrochemical reaction is discharged through the holes in the hole. It is added that the surface of the graphene material 13 is uniformly reacted with the electrolyte S through the pores of the porous filler material 14, and the depth of the reaction can be controlled to be between about 1 mm and 30 mm, preferably 1 mm. Between ~10mm, the thickness of the exfoliated graphene product can be controlled.

Moreover, the porous filler material 14 of the present embodiment may be a porous ceramic plate, a sponge, a foamed plastic, a plastic mesh, a zeolite, a quartz wool or a combination thereof, but is not limited by these materials. Moreover, the porous filler material 14 that can be used and matched in this embodiment can have a pore size of between 5 μm and 1 mm.

The jig 18 is capable of sandwiching the first electrode 11 and the second electrode 12, in other words, the first electrode 11 and the second electrode 12 of the present embodiment are fixed and disposed between the jigs 18. Therefore, through the arrangement of the jig 18, the graphene material 13 of the present embodiment can be fixed and limited between the porous material 14 and the second electrode 12, thereby allowing the graphene material 13 to be completely reacted and achieving a peeling degree of 80%. .

In addition, the graphene generating device 1 of the present embodiment may further include a power supply 15 electrically connected to the first electrode 11 and the second electrode 12, respectively, and generating a potential difference between the first electrode 11 and the second electrode 12. And the power supply 15 can provide direct current or alternating current.

In addition, the graphene generating device 1 of the present embodiment may further include a liquid inlet unit 16 and an exhaust unit (not shown). The liquid inlet unit 16 is used to replenish the electrolyte S, and the exhaust unit is used to discharge the gas generated in the reaction.

In actual operation, the first electrode 11, the second electrode 12, and the porous filler 14 are sequentially mounted in the electrolytic cell 10. Next, the electrolyte S is guided through the pores of the porous filler 14 to bring the electrolyte S into contact with the graphene material 13 on the second electrode 12.

The first electrode 11 and the second electrode 12 have a potential difference. During the reaction, the potential difference causes the electrolyte S to electrolyze and generate hydrogen and oxygen, which are permeable to the porous medium. And the potential difference of this embodiment may be between 5 volts and 100 volts. Preferably, the potential difference can be between 10 volts and 50 volts.

At the same time as the gas is generated, the graphite single layer or the plurality of layers on the surface of the first electrode 11 is expanded and peeled off into a graphene sheet or a graphene powder. The stripped graphene will remain in the electrolytic cell 10. Finally, the stripped graphene is vacuum dried to obtain a product.

The manner in which this embodiment may be matched will be exemplified below.

For example, the graphene material of the present embodiment may be a graphite powder, with a porous filler material 14 of alumina. The average pore diameter of the alumina may be 5 μm, and the thickness of the porous filler 14 of the present embodiment is 5 mm. In other words, the pitch of the first electrode 11 and the second electrode 12 of the present embodiment is 5 mm. The electrolyte was dissolved in 300 ml of 0.25 M sulfuric acid (operating temperature may range from room temperature to 40 ° C). The applied potential difference was 10 V, the current was about 2 A, and about 50 mg of graphene powder was produced at a reaction time of 8 hours.

It should be noted that the pore diameter of the porous filler material 14 of the present embodiment will be selected according to the speed of the electrolyte solution S and the speed of gas escape. In addition, the peeling speed, properties, and yield of graphene can be changed by adjusting the concentration of the electrolyte S, the type of the electrolyte, the type of the solvent, and the potential difference.

Moreover, in other embodiments, the graphene generating device 1 of the present embodiment may further include a filtering and separating product module. The stone of the present embodiment for the purpose of achieving a continuous process The product stripped by the olefin generating device 1 can be passed through a microporous screen of a module for filtering and separating products to filter unpeeled coarse-grained graphite particles, and after screening to obtain a product of an appropriate size (generally thinner than 10 nm) Layer graphene), and then a large amount of deionized water to remove residual electrolyte, or other ionic solution that can dissolve and replace residual ions.

Referring to FIG. 3 and FIG. 4, FIG. 3 is a yield-bar graph of the graphene generating apparatus of the present invention and a conventional electrochemical stripping process. 4 is a thickness distribution-proportional bar graph of a graphene generating apparatus and a conventional electrochemical stripping process of the present invention. 4 is a schematic view showing the thickness distribution of graphene of 500 mesh or less in FIG.

The graph drawn in the drawing is only an embodiment of the present invention, and the porous filler is a porous ceramic plate and can be combined with 0.25 M sulfuric acid as its electrolyte. However, the data may be fine-tuned according to different porous filler materials and electrolytes, but the overall effect between the various embodiments is similar.

For example, the peak of the main yield of the conventional electrochemical stripping mostly falls below 500 mesh, and the peak of the generated thickness is 10-20 nm. In the graphene generating apparatus of the present invention, the peak value of the main yield of graphene will fall below 500 mesh, and the generated thickness mostly falls within the range of 5 to 10 nm. The 5-10 nm graphene product is actually applied and screened out for the subsequent processing. In other words, the graphene production device of the present invention can greatly increase the yield of graphene available in the product, thereby achieving the purpose of improving efficiency and improving overall production quality.

Moreover, the graphene generating device of the present invention has at least the following advantages compared with the conventional electrochemical stripping process. One of the voltages used in the present invention is low, the operating temperature is normal temperature, and the thickness of the product is concentrated in the industry. The standard, the device structure is simple, and the operation is easy, so the present invention can be applied to and meet the requirements of mass production.

Finally, please refer to FIG. 5, which is a side view of a second embodiment of the graphene generating device of the present invention.

Similarly, the graphene generating apparatus 1a of the present embodiment includes an electrolytic cell 10a, at least one first electrode 11a, at least one second electrode 12a, a graphene material 13a, a porous filler 14a, and a jig 18a. And this embodiment also includes a liquid inlet unit 16a.

Different from the foregoing embodiment, there is two, one of the graphene generating devices of the present embodiment 1a has two sets of electrodes, and each set of electrodes includes a first electrode 11a and a second electrode 12a. In other words, the first electrode 11a and the second electrode 12a of the present invention are not limited to one set, and are modularized to combine a plurality of groups in parallel.

Further, the graphene producing apparatus of the present embodiment further includes a screen 17a disposed between the porous filler 14a and the graphene material 13a. The purpose of providing the screen 17a on the first electrode 11a is to prevent the unreacted graphite of the first electrode 11a from entering the porous filler 14a, so that the pores of the porous filler 14a will not be clogged. And the filter 17a can be permeable to enhance the degree of diffusion of the electrolyte.

In addition, the screen 17a of the present embodiment may be disposed between the second electrode 12a and the porous filler 14a. The purpose of the screen 17a is to prevent the graphene material 13a on the second electrode 12a from entering the porous filler 14a. . In short, the filter 17a can be disposed on the surface of the porous filler 14a to improve the overall efficiency of the apparatus.

For example, the graphene material 13a of the present embodiment may be graphite powder, and the porous filler material 14a is a sponge having an average pore diameter of about 1 mm and a thickness of 10 mm (the first electrode 11a and the second electrode 12a of the present embodiment). The pitch is 10mm). The strainer 17a may be a nylon mesh (having a mesh size of about 300 um), and a voltage of 20 V is applied to the first electrode 11a and the second electrode 12a, the current is about 10 A, the total reaction time is 8 hours, and the electrolyte is dissolved in 300 ml. The 0.25 M sulfuric acid solution was combined with 30 ml of potassium hydroxide (30 wt%) and the operating temperature was between room temperature and 40 °C. In this configuration, the yield of graphene is about 500 mg.

In summary, the porous filler material is interposed between the first electrode and the second electrode, and the graphene material is fixed between the second electrode and the porous filler through the jig, and then the porous filler is used to make the electrolyte uniform. The ground reacts with the graphene material on the electrode. Therefore, the present invention can achieve the object of providing a graphene generating device which can be produced at normal temperature, has low cost, improves efficiency, improves overall production quality, and reduces electrode short circuit.

The above is intended to be illustrative only and not limiting. Any equivalent modifications or alterations to the spirit and scope of the invention are intended to be included in the scope of the appended claims.

1‧‧‧graphene generating device

10‧‧‧electrolyzer

11‧‧‧First electrode

12‧‧‧Second electrode

13‧‧‧Graphene materials

14‧‧‧Porous filler

16‧‧‧Inlet unit

18‧‧‧Clamp

S‧‧‧ electrolyte

Claims (9)

A graphene generating device comprising: an electrolytic cell filled with an electrolyte; a clamp; at least one first electrode; at least one second electrode disposed opposite to the first electrode, and the clamp sandwiches the first electrode The second electrode; a graphene material disposed on the second electrode; and a porous filler disposed between the first electrode and the second electrode. The device of claim 1, further comprising a power supply electrically connected to the first electrode and the second electrode, respectively, and causing a potential difference between the first electrode and the second electrode. The device of claim 2, wherein the first electrode and the second electrode have a potential difference, and the potential difference is between 5 volts and 100 volts. The device of claim 3, wherein the potential difference is between 10 volts and 50 volts. The device of claim 1, further comprising a screen disposed between the porous filler and the graphene material. The device of claim 1, wherein the porous filler has a pore size between 5 μm and 1 mm. The device of claim 1, wherein the porous filler material is a porous ceramic plate, a sponge, a foamed plastic, a plastic mesh, a zeolite, a quartz wool, or a combination thereof. The device of claim 1, wherein the first electrode and the second electrode are made of a graphite material or a metal. The device of claim 1, further comprising a liquid inlet unit and an exhaust unit.