AU2018201650B2 - Equipment and/or method(s) for use in graphene production - Google Patents
Equipment and/or method(s) for use in graphene production Download PDFInfo
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- AU2018201650B2 AU2018201650B2 AU2018201650A AU2018201650A AU2018201650B2 AU 2018201650 B2 AU2018201650 B2 AU 2018201650B2 AU 2018201650 A AU2018201650 A AU 2018201650A AU 2018201650 A AU2018201650 A AU 2018201650A AU 2018201650 B2 AU2018201650 B2 AU 2018201650B2
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Abstract
A system 10 for use in electro-chemical exfoliation of graphite to produce
graphene has a housing 12 for holding an electrolysis solution, such as an acid.
Containers 14 within the housing are configured to hold an amount of graphite.
The containers can be baskets constructed primarily of metal, preferably titanium.
Electrodes 18 are placed into the housing adjacent the containers. Mesh and/or
aperture size of each container is between 10 and 200 gauge. A plunger can
maintain contact between the graphite and the container. The plunger can be
actuated by a biasing means (such as a spring) to maintain pressure on the
graphite and in contact with the container side(s)/base. A lid er can act as a
plunger or may have a plunger mounted thereto, which may be manually
actuated. Each container 14 can be in the form of a basket or cage. Side panels
20 and/or end panels 22 and/or a base panel and/or a top panel can each have a
mesh panel 28, 36, 40. A handle 44 may be provided.
16ill
18
100
12
14
Figi1 44
42 26
14 40 A
30 II3
33
228
33
Description
16ill
18
100
12
14
Figi1 44
A 42 26
14 40 II3
33
228
[0001] The present invention relates to equipment and/or methodology for use in producing graphene from graphite.
[0002] Lump graphite (also known as crystalline vein graphite), is a rare and highly valuable material, as it is highest quality naturally occurring graphite product known to man. Such high quality ore is valuable and much sought after for use in steelmaking and even as moderator rods within nuclear reactors.
[0003] Such high quality lump graphite is a valuable resource for the production of graphene. Graphene is an allotrope of carbon in the form of a two dimensional, atomic-scale, hexagonal lattice in which one atom forms each vertex.
[0004] Graphene is the basic structural element of other allotropes of carbon, including graphite, charcoal, carbon nanotubes and fullerenes. It can be considered as an indefinitely large aromatic molecule, the ultimate case of the family of flat polycyclic aromatic hydrocarbons.
[0005] Graphene has 2- dimensional properties, consisting of a single layer of graphite atoms which are tightly packed in a hexagonal pattern. Each atom has four bonds, with an overall sp2 orbital hybridization, and this structure and corresponding forces give rise to a number of extremely useful properties.
[0006] Graphene has many unusual properties. It is reported to be about 200 times stronger than the strongest steel. It efficiently conducts heat and electricity
18672821_1 (GHMatters) P42640AU00 and is nearly transparent. Graphene shows a large and nonlinear diamagnetism, greater than graphite and can be levitated by Neodymium-Iron-Boron (NdFeB) magnets.
[0007] Other properties of graphene include that:
• Graphene is harder than diamonds and stronger than steel.
• Graphene is relatively malleable despite a one atom thick graphene sheet being less than a nanometer thick.
• Graphene is completely impermeable.
• Graphene is a near-perfect thermal conductor.
• Graphene has a variety of highly desirable electronic properties, such as:
a. the highest electrical current density of any known material
b. the highest electron mobility of any known material
c. the lowest resistivity at room temperature of any known materials.
• Graphene is able to self-repair holes in its structure when exposed to carbon-containing molecules.
[0008] It has also been noted that even small amounts of graphene, such as 0.05-2.0% by volume, can impart exponential increases in desirable properties when added to other materials. Therefore, properties of known materials can be
18672821_1 (GHMatters) P42640AU00 modified or optimised for additional or enhanced applications than the base material alone.
[0009] However, these applications are severely limited by the inaccessibility of graphene; even though graphene production has been the subject of much research, and several production facilities have commenced operation in more recent years, isolation of graphene remains a slow and laborious process, with concerns related to quality, efficiency, and cost.
[0010] Known graphene production techniques include: mechanical exfoliation; chemical vapour deposition (CVD); microchemical cleavage (MC); anodic bonding; laser ablation and photo-exfoliation; liquid phase exfoliation (LPE) of graphite; growth on silicon carbide (SiC); and thermal decomposition of graphene films.
[0011] However the use of these methods remains limited and inefficient, due primarily to the fact that the majority of the techniques originate from the production of other minerals.
[0012] For example, in chemical vapour deposition (CVD) it is difficult to identify a substrate on which to grow graphene layers, as well as develop an effective way of removing the graphene layers from the substrate without damaging or modifying their atomic structure.
[0013] The quality of the graphene produced often falls dramatically short of the process' theoretical potential; and processes are associated with negative environmental effects - in particular, the use of toxic and hazardous chemicals which are used during the exfoliation of the mineral can have significant detrimental effects on the environment through their use or poor storage before and after use.
18672821_1 (GHMatters) P42640AU00
[0014] The present invention has been developed in the light of such issues.
[0015] One or more forms of the present invention include(s) equipment and/or methodology for processing graphite to graphene.
[0016] An aspect of the present invention provides equipment for use in the production of graphene from graphite by electro-chemical exfoliation of the graphite, the equipment including a container for supporting graphite within an electrolytic solution, the container including at least one side and a base and a first electrode for the electro-chemical exfoliation process, wherein the at least one side includes a plurality of side panels and a plurality of end panels.
[0017] Preferably, the container includes a mesh. The mesh may form the at least one side and/or base of the container.
[0018] The container may be partially made of metal. Preferably the metal includes titanium or is titanium.
[0019] The container may be a basket or cage primarily of metal and/or of metal and polymer.
[0020] The polymer may include polyethylene, polycarbonate or polypropylene, or combinations of two or more thereof.
[0021] The at least one side may include a plurality of side panels and a plurality of end panels.
[0022] The side panels may be disposed opposite one another, and the end panels may be disposed opposite one another, and the opposed side and
18672821_1 (GHMatters) P42640AU00 opposed end panels connected to form a multi-sided structure and connected to the base.
[0023] The at least one side and/or the base may be electrically conductive providing the electrode.
[0024] The equipment may include at least one terminal for connecting the container to an electrical supply.
[0025] The equipment may include a housing for containing the acid solution, and the container may be disposed within the housing.
[0026] Graphite put within the container preferably contacts the at least one side and/or base that provides the first electrode. The electrolysis solution may provide a second electrode of opposite electrical polarity to the first electrode.
[0027] The container and the graphite therein preferably act as an anode in the electrolysis process.
[0028] Preferably the electrolysis solution is in contact with at least one cathode in the electrolysis process.
[0029] The at least one cathode may be provided by at least one metal plate or mesh supported in the electrolysis solution.
[0030] The graphite may include crystalline vein graphite as part of the anode or other forms of graphite.
[0031] Preferably, the electrolysis solution includes at least one acid, such as one or more of hydrochloric acid (HCI), nitric acid (HNO3) or sulphuric acid (H2SO4) or citric acid (C6H807).
18672821_1 (GHMatters) P42640AU00
[0032] The container may include mesh retained thereto. The mesh may be titanium.
[0033] Preferably the container includes the at least one side with apertures therethrough, and the mesh applied externally of the container.
[0034] The container may include multiple side panels and/or end panels retained together with fasteners. Preferably the fasteners are made of titanium.
[0035] The fasteners may include bolts and nuts fastening the side panels and/or end panels together. The base may be fastened to the side panels and/or end panels.
[0036] The container may include a top panel, which may include apertures therethrough and may include an optional mesh.
[0037] One or more retainers may be provided to retain the mesh to the respective side and/or end panels. The one or more retainers may clamp the mesh to the respective side and/or end panels.
[0038] The container may include attachment means for supporting the container within the housing holding the electrolysis solution.
[0039] One or more forms of the present invention will hereinafter be described with reference to the accompanying figures, in which:
[0040] Figure 1 shows an arrangement of electro-chemical production equipment including two containers for holding graphite within a housing to hold
18672821_1 (GHMatters) P42640AU00 an acid solution for producing graphene by electro-exfoliation according to an embodiment of the present invention.
[0041] Figure 2 shows an exploded view of a container for holding graphite for producing graphene during an electro-chemical exfoliation process according to an embodiment of the present invention.
[0042] As shown in figure 1, a system 10 for use in electro-chemical exfoliation of graphite to produce graphene includes a housing 12 for holding an electrolysis solution.
[0043] The electrolysis solution can be an acid solution, such as containing sulphuric acid, hydrochloric acid or nitric acid.
[0044] The electrolysis solution can be a weak acidic solution, such as up to % acid by volume in water, more preferably up to 7.5% and yet more preferably up to 5%.
[0045] A pair of containers 14 is disposed within the housing, each of the containers configured to hold an amount of graphite, preferably crystalline vein graphite.
[0046] The containers are preferably constructed primarily of metal, most preferably titanium. Significant research and testing has found that, unexpectedly, titanium is a preferred choice for the containers of the present invention.
[0047] An electrical connection is 16 provided to each of the containers. Electrodes 18 are placed into the housing adjacent the containers.
18672821_1 (GHMatters) P42640AU00
[0048] In use, an electrical current is passed through the acid solution between the graphite in contact with the containers 14 and the electrode(s) 18 to electro-chemically exfoliate graphene from the graphite.
[0049] It will be appreciated that impurity elements within the graphite ore, such as silicon, iron (from magnetite), calcium, magnesium, aluminium and phosphorus oxides can help with intercalation (along with anions/cations of the electrode that is not the graphite) and separation of layers of graphene from the host graphite.
[0050] The electro-chemical exfoliation equipment helps to: eliminate the requirement for initial crushing and grinding of graphite, as currently done in other production processes and to produce graphene of various micron sizes for selectable and tailored use in a variety of applications.
[0051] Electro-chemical exfoliation is a known technique used in materials processing which makes use of ion flow through an electrolytic solution. The raw material which is to be refined can be positively or negatively charged when connected to a power source. This causes it to act as either a "cathode" or an "anode" depending on its net charge - it becomes a cathode if positively charged by the power source, or an anode if negatively charged.
[0052] The electrochemical reaction then progresses depending on which charge this source material carries. Free ions from the non-graphite electrode will flow through the electrolytic solution in a direction determined by the principles of electromagnetic attraction and repulsion - with oppositely charged ions attracted to the raw material. As such, the process requires that the ions present and graphite be oppositely charged.
[0053] The charge applied to the graphite within the container(s) is thus chosen depending on the valency of the material being used for the other
18672821_1 (GHMatters) P42640AU00 electrode. Lithium, for example, has a valency of +1, meaning that it produces positive ions, or cations. This is because it only has one valence electron, and it is therefore more efficient for lithium atoms to lose this single electron, shedding its now empty shell to make its full shell beneath it its stable outer shell - and a positive charge, since it lost a negatively-charged particle.
[0054] For example, if lithium is used for the cathode electrode, then graphite would be made the anode electrode, and cations of the lithium would flow through the electrolytic solution towards the graphite - since they are attracted to the now negatively charged material. These cations then intercalate, or 'insert' themselves, between one or more sheets of the raw material. By wedging themselves between layers, more cations can bond with the material due to the increased surface area. As this occurs, sheets of the material peel away from the source block and can be collected.
[0055] The equipment may include thermal control of the temperature of the electrolysis solution. The housing may be provided with a lid to retain heat.
[0056] Preferably the mesh and/or aperture size of the container is of a mesh between 10 and 200 gauge, preferably between 20 and 100 gauge., and more preferably between 20 and 40 gauge, and yet more preferably at substantially 30 gauge.
[0057] Preferably, impurities, such as silicon, are removed, such as during the graphene production process. Silicon can be extracted by flushing from capture as it collects at the internal floor of the housing.
[0058] The electric current through the electrolysis solution can dramatically drops during continuous graphene production if there is a reduction or loss of contact between the graphite ore and electrode(s) provided by the container(s).
18672821_1 (GHMatters) P42640AU00
[0059] A plunger-like component can be provided to help maintain contact between the graphite and the container. The plunger can be actuated by a biasing means (such as a spring) to maintain pressure on the graphite and in contact with the container side(s)/base. Alternatively, or in addition, a lid of the container may act as a plunger or may have a plunger mounted thereto, which may be manually actuated.
[0060] As shown in Figure 2 by way of example, the container 14 can be in the form of a basket or cage. The opposed side panels 20 have apertures allowing the electrolysis solution to contact the graphite and to increase surface area of the sides compared with solid sheet sides.
[0061] The side panels 20 are retained in spaced relationship by connection to two opposed end panels 22. A base panel 24 forms the floor of the container. Preferably the side panels, end panels and base have apertures.
[0062] A top panel 26 can be provided to enclose graphite within the container, but is optional.
[0063] The side panels 20 can have a mesh panel 28 fastened thereto, such as by retainers 30. Likewise, the end panels 22 can have mesh panels 32 retained thereto, such as by retainers 34.
[0064] A mesh panel 36 can be retained to the base by a retainer 38. Likewise, a mesh panel 40 can be retained to the top panel by a retainer 42. A handle 44 can be provided, which may form part of or be attached to the retainer 42.
[0065] It is to be understood that, if any prior art publication is referred to herein, such reference does not constitute an admission that the publication
18672821_1 (GHMatters) P42640AU00 forms a part of the common general knowledge in the art, in Australia or any other country.
[0066] In the claims which follow and in the preceding description of the invention, except where the context requires otherwise due to express language or necessary implication, the word "comprise" or variations such as "comprises" or "comprising" is used in an inclusive sense, i.e. to specify the presence of the stated features but not to preclude the presence or addition of further features in various embodiments of the invention.
18672821_1 (GHMatters) P42640AU00
Claims (21)
1. Equipment for use in the production of graphene from graphite by electro-chemical exfoliation of the graphite, the equipment including a container for supporting graphite within an electrolytic solution, the container including at least one side and a base and a first electrode for the electro-chemical exfoliation process, wherein the at least one side includes a plurality of side panels and a plurality of end panels.
2. The equipment of claim 1, wherein the container includes a mesh.
3. The equipment of claim 2, wherein the mesh forms the at least one side and/or base of the container or is provided as a mesh retained to the at least one side and/or base.
4. The equipment of any one of claims 1 to 3, wherein the container is at least partially made of metal.
5. The equipment of claim 4, wherein the metal includes titanium or is titanium.
6. The equipment of claim 1, wherein the container includes a basket or cage primarily of metal and/or of metal and polymer.
7. The equipment of claim 6, wherein the polymer includes polyethylene, polycarbonate or polypropylene, or combinations of two or more thereof.
8. The equipment of any one of the preceding claims, wherein the at least one side and/or the base is/are electrically conductive providing the electrode in contact with the graphite
18672821_1 (GHMatters) P42640AU00
9. The equipment of any one of the preceding claims, including a housing for containing the electrolysis solution, and the container disposed within the housing during graphene production.
10. The equipment of claim 8, wherein graphite put within the container contacts the at least one side and/or base that provides the first electrode.
11. The equipment of any one of the preceding claims, wherein the electrolysis solution includes at least one acid.
12. The equipment of claim 11, wherein the at least one acid includes one or more of hydrochloric acid (HCI), nitric acid (HNO3),sulphuric acid (H2SO4) or citric acid (C6H807).
13. The equipment of any one of the preceding claims, wherein the container includes mesh.
14. The equipment of claim 13, wherein the mesh is titanium or includes titanium.
15. The equipment of claim 13 or claim 14, wherein the mesh forms at least one of the said side(s) and/or base or is retained to the said side(s) and/or base.
16. The equipment of claim 1, wherein the at least one side and/or base include(s) apertures.
17. The equipment of any one of the preceding claims, wherein the at least one side and/or base are retained together by fasteners.
18. The equipment of claim 17, wherein the fasteners are of titanium or include titanium.
18672821_1 (GHMatters) P42640AU00
19. The equipment of claim 18, wherein the fasteners include bolts.
20. The equipment of any one of the preceding claims, including at least one device for biasing the graphite into contact with the at least one side and/or base of the container.
21. The equipment of claim 20, wherein the device includes a plunger.
18672821_1 (GHMatters) P42640AU00
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2017900825 | 2017-03-09 | ||
| AU2017900825A AU2017900825A0 (en) | 2017-03-09 | Equipment and/or method(s) for use in graphene production |
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| Publication Number | Publication Date |
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| AU2018201650A1 AU2018201650A1 (en) | 2018-09-27 |
| AU2018201650B2 true AU2018201650B2 (en) | 2022-06-09 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090028778A1 (en) * | 2007-07-27 | 2009-01-29 | Aruna Zhamu | Environmentally benign graphite intercalation compound composition for exfoliated graphite, flexible graphite, and nano-scaled graphene platelets |
| US20130161199A1 (en) * | 2011-12-23 | 2013-06-27 | Academia Sinica | Production of Graphene |
| US20160186341A1 (en) * | 2014-12-25 | 2016-06-30 | National Taiwan Normal University | Apparatus and method for producing a graphene material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090028778A1 (en) * | 2007-07-27 | 2009-01-29 | Aruna Zhamu | Environmentally benign graphite intercalation compound composition for exfoliated graphite, flexible graphite, and nano-scaled graphene platelets |
| US20130161199A1 (en) * | 2011-12-23 | 2013-06-27 | Academia Sinica | Production of Graphene |
| US20160186341A1 (en) * | 2014-12-25 | 2016-06-30 | National Taiwan Normal University | Apparatus and method for producing a graphene material |
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| AU2018201650A1 (en) | 2018-09-27 |
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