Stack reactor for batch graphite intercalation

Abstract

The present invention relates to a reactor for intercalating a graphite material, comprising an expandable reaction chamber to allow for expansion of said graphite material during intercalation. The reactor comprises a fluid permeable cathode plate with a fluid permeable separator, and a fluid permeable anode plate. At least one of the cathode and anode plates is biased towards the graphite in the reactor by a biasing element, and is moveably arranged to allow for expansion of the graphite material.

Description

[0001] 83369PC01

[0002] 1

[0003] STACK REACTOR FOR BATCH GRAPHITE INTERCALATION

[0004] FIELD OF THE INVENTION

[0005] The present invention relates to a reactor for intercalating a graphite material, comprising an expandable reaction chamber to allow for expansion of said graphite material during intercalation. The reactor comprises a fluid permeable cathode plate with a fluid permeable separator, and a fluid permeable anode plate. At least one of the cathode and anode plates is biased towards the graphite in the reactor by a biasing element, and is moveably arranged to allow for expansion of the graphite material.

[0006] BACKGROUND OF THE INVENTION

[0007] Intercalation is a process in which molecules and / or ions are inserted between layers of layered materials, such as in between graphene layers of graphite as in the present invention, resulting in molecules or ions being embedded in between the graphene layers and increased interlayer distance in the graphite. This is typically performed to achieve an intercalated graphite material with specific properties, such as specific electrical properties or to achieve properties of an active material. Increasing the interlayer distance by driving the molecules or ions into the layered graphite requires energy, and providing that energy can be done through both chemical and physical processes. These processes can for example include transfer of charges between the molecules or ions and the graphene layers, or use of sufficiently strong electric fields for driving the molecules or ions into interlayer positions.

[0008] To perform the intercalation process using electric fields, contact needs to be kept between an anode producing the electric field and the graphite material. As the volume of the graphite changes during the process this becomes a problem, as the contact area between the graphite and the anode may reduce or the graphite can move out of contact with the anode. Hence, an improved reactor that ensures that contact remains between the graphite and the anode during the process would be advantageous, and in particular a more compact reactor without externally moving parts would be advantageous. 83369PC01

[0009] 2

[0010] OBJECT OF THE INVENTION

[0011] It is an object of the invention to provide an efficient reactor for intercalation of graphite which eliminates the use of externally moving parts and ensures reliable process control by maintaining contact between the anode and the graphite material during the intercalation process.

[0012] It is a further object of the present invention to provide an alternative to the prior art.

[0013] SUMMARY OF THE INVENTION

[0014] Thus, the above described object and several other objects are intended to be obtained in a first aspect of the invention by providing a reactor for intercalating a graphite material, comprising

[0015] • an expandable reaction chamber configured to retain an amount of graphite material and to allow for expansion of said graphite material during intercalation, wherein said expandable reaction chamber being a first void interior of said reactor, said void being defined at least by:

[0016] - a fluid permeable cathode plate comprising a cathode outward surface and a cathode inward surface, said cathode inward surface facing said first void,

[0017] - a fluid permeable separator arranged between said cathode inward surface and said graphite material,

[0018] - a fluid permeable anode plate comprising an anode outward surface and an anode inward surface, said anode inward surface facing said first void,

[0019] - one or more wall elements arranged to provide said void in combination with said cathode plate and said anode plate,

[0020] - wherein said cathode plate with said fluid permeable separator and / or said anode plate is / are moveably arranged so that an expansion of said expandable chamber is provided by movement of said cathode plate and / or said anode plate,

[0021] • a biasing member for biasing said cathode plate and / or said anode plate towards said void by providing a force against said cathode plate outward surface and / or said anode plate outward surface in the direction of said void, 83369PC01

[0022] 3

[0023] • a first back member arranged opposite said cathode plate outward surface or anode plate outward surface for providing an opposing force to said biasing member,

[0024] • at least one electrolyte supplying conduit arranged to supply an electrolyte fluid to said void from an exterior of said reactor, said electrolyte supplying conduit comprising at least one electrolyte inlet and at least one electrolyte outlet.

[0025] Terms are used herein in a manner being ordinary to the skilled person. Some of the used terms are elucidated here below:

[0026] Plane as used in cathode and anode plate preferably refers to a two-dimensional space spanned by the two longest of the width, height and length of the cathode or anode plate.

[0027] Retain as used in "an expandable reaction chamber (8) configured to retain the graphite material" preferably refers to holding entirely within in a manner which allows for no escape of the specified material.

[0028] Spatial orientation as used in "predetermined spatial orientation of said cathode plate (6) with said separator (7) or said anode plate (10)" preferably refers to the orientation of the cathode plate or anode plate in relation to the device, such as the angles between surface normals of said cathode plate or anode plate. A predetermined spatial orientation is typically kept the same during movement of the cathode plate, and when implemented the separator, and / or the anode plate.

[0029] Stacked configuration / arrangement as used herein preferably refers to a reactor where the elements of the reactor are arranged in a stacked manner and the reactor preferably has no externally moving parts.

[0030] BRIEF DESCRIPTION OF THE FIGURES

[0031] The present invention and in particular preferred embodiments thereof will now be described in more detail with regard to the accompanying figures. The figures show various embodiments of the present invention and are not to be construed 83369PC01

[0032] 4 as being limiting to other possible embodiments falling within the scope of the attached claim set.

[0033] Fig. la illustrates a three-dimensional view of the exterior of a first and a second embodiment of a reactor. Fig. lb illustrates in a cross sectional view a cross section of the first embodiment of the reactor illustrated in Fig. la. Fig. lc illustrates in a cross sectional view a cross section of the second embodiment of the reactor illustrated in Fig. la. The cross sectional views are along the dashed line illustrated in Fig. la.

[0034] Fig. 2a illustrates a 3-dimensional view of the exterior of a third embodiment of a reactor. Fig. 2b illustrates in a cross sectional view a cross section of the third embodiment of the reactor illustrated in Fig. 2a. The cross sectional view is along the dashed line illustrated in Fig. 2a.

[0035] DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS

[0036] Reference is made to Fig. lb illustrating a cross section view of a first embodiment of a reactor. The reactor is configured for intercalating a graphite material, preferably by having an expandable reaction chamber with an electric field and an influx of electrolyte containing molecules or ions for intercalation. Graphite material used in connection with preferred embodiments of the invention may be any form of material consisting of stacked layers of carbon in the form of graphene. The graphite can be provided to the reactor in a plurality of different forms, such as in the form of flakes or granules.

[0037] Intercalation of graphite in connection with the present invention is the introduction of molecules or ions between the layers of graphene of the graphite material. The introduction of the molecules or ions in the graphite increases the distance between the graphene layers, resulting in an expansion of the graphite material. The molecules or ions are preferably driven into the graphite material by an electric field. The molecules or ions can include, but are not limited to, molecules or ions of lithium, potassium, fluorine, caesium or ytterbium.

[0038] Specifically, Fig. lb illustrates a cross section along the dashed line in Fig. la of a first embodiment of a reactor for intercalating a graphite material, comprising an 83369PC01

[0039] 5 expandable reaction chamber 8. The expandable reaction chamber 8 is arranged to define a void of the reaction chamber 8, and hold therein a graphite material to be intercalated. The void of the reaction chamber 8 is a volume, such as a substantially rectangular cuboid-shaped volume, although the void may be in other forms, and is expandable to adapt the volume of the void to the increasing volume of a graphite material that expands during an intercalation process

[0040] In the first embodiment, graphite material is held in the void of the reaction chamber 8 by impermeable wall elements 81, a cathode 6 and an anode 10 both in the form of plates with a fluid permeable structure, such as an open pore structure or a perforated structure. The openings of the fluid permeable cathode 6 and anode 10 plates are large enough to allow flow of electrolyte and smaller particles, such as small graphite or graphene particles, therethrough, but too small to allow larger particles, such as larger pieces of graphite, from escaping the void of the reaction chamber. An inward surface 6b of the cathode plate 6 and an inward surface 10b of the anode plate 10 are arranged facing each other, on opposite sides of the graphite material within the void of the reaction chamber.

[0041] In preferred embodiments, the openings of the fluid permeable cathode plate 6 and / or the fluid permeable anode plate 10 are large enough to allow flow of electrolyte therethrough, but small enough that graphite and graphene material of a predetermined minimum size, e.g. larger than 20 nm, are prevented from escaping the void of the reaction chamber.

[0042] In preferred embodiments where separators 7, 11 are arranged to prevent graphite and graphene material of a predetermined minimum size, e.g. larger than 20 nm, from escaping the void of the reaction chamber 8 the size of the openings of the fluid permeable cathode plate 6 and / or the fluid permeable anode plate 10 may be in the range of 10 pm to 10 mm.

[0043] In preferred embodiments a fluid permeable separator 7 is arranged to cover at least partly, such as fully, the inward surface 6b of the cathode plate 6 to prevent electrical contact between the cathode plate 6 and the graphite material. The openings of the fluid permeable separator 7 are large enough to allow flow of electrolyte therethrough, but small enough that graphite and graphene material of 83369PC01

[0044] 6 a predetermined minimum size, e.g. larger than 20 nm, are prevented from escaping the void of the reaction chamber. The inward surface 10b of the anode plate 10 is arranged in electrical contact with the graphite material, such that the graphite material behaves electrically as part of an anode.

[0045] In the first embodiment, the cathode plate 6 with the separator 7 is arranged in a non-moveable position within the reactor. A biasing member 13, such as a compression spring, is arranged between an outward surface 10a of the anode plate 10 and a first back member 3a, biasing the anode plate 10 towards the graphite material arranged in the void of the reaction chamber 8 to maintain electrical contact between the graphite material and the anode plate 10. In a preferred embodiment, the cathode plate 6 is fixedly arranged by an edge of the cathode plate 6 being received in a slot or slots of one or more of the wall members 81, so that the cathode plate 6 with the separator are in a non- moveable position within the reactor.

[0046] In some embodiments, the separator 7 may be arranged parallel to and at a distance from the cathode plate 6 such that a void is defined between the cathode plate 6 and the separator 7. As the separator 7 is substantially non-permeable to the graphite material, the void between the cathode 6 and the separator 7 is configured to be a substantially graphite-free void. Preferably, the distance between the cathode plate 6 and the separator 7 is large enough to ensure that any small graphite particles which may pass through the separator are not able to be in simultaneous contact with the cathode plate inward surface 6b and the separator 7. In such embodiments, it may be determined that a leakage of graphite material through the separator 7 has occurred by detecting a presence of graphite material in the void between the cathode 6 and separator 7.

[0047] In preferred embodiments, the biasing member 13 comprises at least one compression spring. Typically, such a spring is a coiled member made of spring steel, or a non-conductive material. Alternatively, the coiled member may be made from spring steel and coated by a non-conductive coating. A compression spring is typically a spring which can be compressed, and in preferred embodiments, the compression spring is in the form of an open helix. 83369PC01

[0048] 7

[0049] Alternatively, the biasing member is in the form of a pneumatic spring, wherein the spring force is provided by compression of a gas, such as inert gas or air.

[0050] The anode plate 10 in the first embodiment is arranged to be able to move in at least one direction, such as a direction away from the void of the reaction chamber, so that movement of the anode plate 10 results in expansion of the volume of the void of the reaction chamber 8 and compression of the biasing member 13. The movement of the anode plate 10 is caused by the expanding graphite material during intercalation exerting a force on the inward surface 10b of the anode plate such that the void of the reaction chamber 8 expands together with the graphite material. The force on the inward surface 10b results in compression of the biasing member 13.

[0051] The reactor according to the first embodiment further comprises an electrolyte supplying conduit 1 which comprises an electrolyte inlet la preferably being an opening exterior to said reactor, such as an opening in the wall elements 81, arranged to allow an electrolyte to flow into the reactor and the reaction chamber 8, through the cathode plate 6 or anode plate 10, and an electrolyte outlet lb preferably being another opening exterior to said reactor, such as an opening in the wall elements 81, arranged to allow the electrolyte to exit the reactor. In the embodiments illustrated in the figures, the electrolyte inlet and outlet la, lb are provided by connecting pipes.

[0052] In preferred embodiments, the electrolyte is preferably a liquid electrolyte, such as an aqueous or a non-aqueous liquid electrolyte comprising sulphates, perchlorates and / or nitrates for intercalating the graphite material.

[0053] In the first embodiment the electrolyte inlet la is arranged to flow electrolyte towards the outward surface 6a of the cathode plate 6 resulting in that electrolyte flowing from the electrolyte inlet la passes through the cathode plate 6 and the separator 7 to enter the void of the reaction chamber 8. The electrolyte outlet lb is arranged so that electrolyte from the void of the reaction chamber 8 passes through the separator 7 and the cathode plate 6 to exit the reactor. 83369PC01

[0054] 8

[0055] Although the flow direction of the electrolyte in the illustrated embodiment is disclosed through an upper inlet la and a lower outlet lb, the flow direction of electrolyte can be reversed, such that electrolyte flows from the electrolyte outlet lb (hence being an inlet), through the cathode plate 6 and the separator 7 into the void of the reaction chamber 8 and leaves the void of the reaction chamber 8 by flowing through the separator 7 and the cathode plate 6 and exits the reactor through the electrolyte inlet la (hence being an outlet). Alternatively, the electrolyte can flow from one of the electrolyte inlet la or the electrolyte outlet lb, flow through the cathode plate 6, and exit through the other of the electrolyte inlet la or the electrolyte outlet lb.

[0056] In some embodiments, the electrolyte inlet la and / or the electrolyte outlet lb may be arranged in direct fluid communication with the reaction chamber 8 such that electrolyte flowing into the electrolyte inlet la flows directly into the reaction chamber 8, and / or electrolyte flows into the electrolyte outlet lb directly from the reaction chamber 8.

[0057] The movement of the anode plate 10 in the first embodiment is preferably a substantially linear translation along an axis, wherein the axis is an axis substantially parallel to the normal of a plane, wherein the plane can be defined by, but is not limited to, a plane substantially parallel to the inward surface 10b and / or the outward surface 10a of the anode plate 10, a plane substantially parallel to the inward surface 6b and / or the outward surface 6a of the cathode plate 6, a plane substantially perpendicular to surfaces of the wall elements 81 which define boundaries of the void of the reaction chamber 8 or a plane defined by any combination thereof.

[0058] A cross section along the dashed line in Fig. la of a second embodiment of the reactor is illustrated in Fig. lc. Many features of the second embodiment are similar to those as described in regard to the first embodiment as apparent from the Fig. la and Fig. lb. The second embodiment differs, inter alia, from the first embodiment in that the anode plate 10 is arranged in a non-moveable position within the reactor. The biasing member 13, is arranged between an outward surface 6a of the cathode plate 6 and a first back member 3a, biasing the cathode plate 6 and the separator 7 towards the graphite material in the void of the 83369PC01

[0059] 9 reaction chamber 8 to maintain electrical contact between the graphite material and the anode plate 10. In a preferred embodiment, the anode plate 10 is fixedly arranged by an edge of the anode plate 10 being received in a slot or slots of one or more of the wall members 81, so that the anode plate 10 is in a non-moveable position within the reactor.

[0060] In the second embodiment the cathode plate 6 with the separator 7 is arranged to be able to move in a direction away from the void of the reaction chamber such that movement of the cathode plate 6 results in expansion of the volume of the void of the reaction chamber 8 and compression of the biasing member 13. The movement of the cathode plate 6 with the separator 7 is caused by the expanding graphite material during intercalation exerting a force on the inward surface 6b of the cathode plate 6 with the separator 7 such that the void of the reaction chamber 8 expands together with the graphite material. The force on the inward surface 6b results in compression of the biasing member 13.

[0061] The movement of the cathode plate 6 with the separator 7 in the second embodiment is preferably a substantially linear translation along an axis, wherein the axis is an axis substantially parallel to the normal of a plane, wherein the plane can be defined by, but is not limited to, a plane substantially parallel to the inward surface 10b and / or the outward surface 10a of the anode plate 10, a plane substantially parallel to the inward surface 6b and / or the outward surface 6a of the cathode plate 6, a plane substantially perpendicular to surfaces of the wall elements 81 which define boundaries of the void of the reaction chamber 8 or a plane defined by any combination thereof.

[0062] In the second embodiment the electrolyte inlet la being arranged to flow electrolyte towards the outward surface 10a of the anode plate 10 resulting in that electrolyte flowing from the electrolyte inlet la passes through the anode plate 10 to enter the void of the reaction chamber 8. The electrolyte outlet lb is arranged so that electrolyte from the void of the reaction chamber 8 passes through the anode plate 10 to exit the reactor.

[0063] Although the flow direction of the electrolyte in the illustrated embodiment is disclosed through an upper inlet la and a lower outlet lb, the flow direction of 83369PC01

[0064] 10 electrolyte can be reversed, such that electrolyte flows from the electrolyte outlet lb (hence being an inlet), through the anode plate 10 into the void of the reaction chamber 8 and leaves the void of the reaction chamber 8 by flowing through the anode plate 10 and exits the reactor through the electrolyte inlet la (hence being an outlet). Alternatively, the electrolyte can flow from one of the electrolyte inlet la or the electrolyte outlet lb, through the anode plate 10, and exit through the other of the electrolyte inlet la or the electrolyte outlet lb.

[0065] Reference is made to Fig. 2b, which illustrates a cross section along the dashed line of Fig. 2a of a third embodiment of a reactor. In the third embodiment, the wall elements 81 comprise a second back member 3b, impermeable reaction chamber wall elements 82, and impermeable expansion space wall elements 83. The reaction chamber wall elements 82 are arranged to define walls of the void of the reaction chamber 8. The inward surface 10b of the anode plate 10, and the inward surface 6b of the cathode plate 6 with the separator 7 define the remaining walls of the reaction chamber.

[0066] In the third embodiment, the expansion space wall elements 83 are arranged to define walls of expansion space 9 being a void separate from the void of the reaction chamber. Remaining walls of the expansion space are defined by the outward surface 10a of the anode plate 10 and the first back member 3a. The expansion space 9 is arranged to decrease in volume in response to an increase in volume of the void of the reaction chamber 8. The decrease in volume of the expansion space 9 preferably has a linear relation to the increase in volume of the void of the reaction chamber 8, such as the decrease in volume of the expansion space 9 being equal in magnitude to the increase in volume of the void of the reaction chamber, or the volumetric decrease of the expansion space 9 being equal in magnitude to the volumetric increase of the reaction chamber 8 times a constant. Alternatively, the expansion space 9 can increase in volume in response to a decrease in volume of the void of the reaction chamber 8.

[0067] In preferred embodiments the parts of the reactor, which can include, but are not limited to, the wall elements 81, being any one of the wall elements 81 as described for embodiment 1 or the wall elements 81 comprising the second back member 3b, the reaction chamber wall elements 82 and the expansion space wall 83369PC01

[0068] 11 elements 83, the cathode plate 6 with the separator 7, the anode plate 10, the reaction chamber 8, the expansion space 9, the biasing member 13 and the first back member 3a, are held together in the reactor in a stacked configuration. The stacked configuration is preferably a configuration wherein surfaces of adjacent parts abut to provide substantially gap-free interfaces, such as interfaces which inhibit or fully prevent electrolyte, purging fluid and / or graphite material to pass through the interfaces.

[0069] In preferred embodiments the reactor is held together in the stacked configuration by a clamping arrangement, where the clamping arrangement comprises at least two clamping members 2 arranged on opposite sides of the stacked arrangement, such as arranged in abutment with opposite external surfaces of the wall elements 81 and the first back member 3a or in abutment with external surfaces of the first 3a and second 3b back members. The two clamping members 2 are preferably arranged to distribute a clamping force from a clamping device over the opposite external surfaces of the reactor. Alternatively, the clamping members 2 comprise openings or protrusions for receiving clamping surfaces of the clamping device or for engaging with and serving as a part of the clamping device.

[0070] In preferred embodiments the clamping device is a device that can be attached over the reactor to provide a force to each one of the clamping members 2 to maintain the reactor in stacked configuration. Typically, the clamping device is one of a bar clamp, a pipe clamp, a band clamp or a vise. Alternatively, the clamping device comprises connecting members, such as threaded rods or nuts and bolts, for engaging with the openings or protrusions in the clamping members to form a clamping connection between the clamping members 2, wherein the openings or protrusions preferably comprise threaded openings for engaging with threads on threaded rods, and / or non-threaded openings to receive bolts, where ends of the bolts can be fitted with nuts, where the nuts can be tightened or loosened on the bolts in order to increase or decrease the force exerted on the clamping members 2 by the clamping arrangement.

[0071] In some embodiments, the reactor may be held together in the stacked configuration by affixing of abutting elements. For example, the wall elements 81 and the first back member 3a may be fixed to each other, or the first back 83369PC01

[0072] 12 member 3a may be fixed to the expansion space wall elements 83, the expansion space wall elements 83 may be fixed to the reaction chamber wall elements 82, and the reaction chamber wall elements 82 may be fixed to the second back member 3b. In such embodiments, clamping members 2 may be provided for additional clamping of the elements, or the clamping members 2 may be provided for holding the stack reactor in a fixed position.

[0073] By providing a reactor in a stacked configuration, all moving parts of the reactor are retained internally within the reactor, and the reactor preferably has no externally moving parts. This increases the safety of the reactor, inter alia by minimizing leakages and increasing safety in handling. Simultaneously, the dimensions of the reactor are kept constant and the required space for the reactor is predictable.

[0074] In the third embodiment a further separator 11 is arranged to cover at least partly, such as fully, the outward surface 10a of the anode plate 10 to prevent graphite from entering into the expansion space 9 from the void of the reaction chamber 8 through the anode plate 10. The biasing member 13 is arranged between the further separator 11 on the outward surface 10a of the anode plate 10 and the first back member 3a in order to bias the anode plate 10 with the further separator 11 against the graphite material within the void of the reaction chamber, and to maintain contact between the graphite material and the inward surface 10b of the anode plate 10. The first back member 3a is fixedly arranged to provide an opposing force to the biasing member 13 such that the biasing member exerts a constant force on the outward surface 10a of the anode plate 10 with the further separator 11. Use of the further separator 11 is not limited to the third embodiment and may be implemented in other embodiments of the invention, such as in the first and / or second embodiment(s).

[0075] In preferred embodiments, the further separator 11 has a fluid permeable structure, such as a perforated structure or a membrane structure, wherein the openings of the fluid permeable further separator 11 are large enough to allow electrolyte to flow therethrough and small enough to prevent graphene and graphite material of a predetermined minimum size, e.g. larger than 20 nm, from passing through the further separator 11 into the expansion space 9. 83369PC01

[0076] 13

[0077] In preferred embodiments, the fluid permeable further separator 11 is made of a non-conducting material. The further separator 11 can be arranged to serve as an electrical insulator to prevent electrical contact between the anode plate 10 and the biasing member 13, and / or to prevent electrical contact between the graphite material and the biasing member 13.

[0078] In the third embodiment, the electrolyte supplying conduit 1 further comprises a fluid distribution element 5 which is arranged between the second back member 3b and the outward surface 6a of the cathode plate 6. The fluid distribution element 5 is fluidica lly connected to the electrolyte inlet la and the electrolyte outlet lb so that electrolyte entering through the electrolyte inlet la or electrolyte outlet lb flows through the fluid distribution element 5 and is distributed, such as evenly distributed, over the surface 6a of the cathode plate 6. Use of the fluid distribution member 5 is not limited to the third embodiment and may be implemented in other embodiments of the invention, such as in the first and / or second embodiment(s).

[0079] Alternatively, the fluid distribution element 5 may in some embodiments be arranged between the cathode inward surface 6b and the separator 7 such that when the electrolyte flows from the electrolyte inlet la to the reaction chamber 8, the electrolyte flows through the cathode 6, the fluid distribution element 5 and then the separator 7 in order, and when the electrolyte flows from the reaction chamber 8 to the electrolyte outlet, the electrolyte flows through the separator 7, the fluid distribution element 5 and the cathode 6 in order.

[0080] In preferred embodiments, the electrolyte supplying conduit 1 is arranged in, such as through or as a part of, the wall elements 81 or the second back member 3b. The electrolyte inlet la and the electrolyte outlet lb of the electrolyte supplying conduit 1 can for example be provided by connecting pipes arranged within through-holes of the wall elements 81 or the second back member 3b, through- holes of the wall elements 81 or the second back member 3b, and / or hollow tubular protrusions on the wall elements 81 or the second back member 3b. 83369PC01

[0081] 14

[0082] In preferred embodiments the electrolyte inlet la and the electrolyte outlet lb are arranged to be accessed from an exterior of the reactor, so that electrolyte for intercalating the graphite material can be provided to the void of the reaction chamber 8 from an exterior of the reactor through the electrolyte inlet la and / or the electrolyte outlet. Preferably connection points of the electrolyte inlet la and the electrolyte outlet lb for providing fluid communication with an electrolyte supply are provided flush with and on or protruding from an exterior surface of the reactor, such as a surface of the wall elements 81 or the second back member 3b.

[0083] In the third embodiment the reactor further comprises at least one purging conduit 16, where the purging conduit 16 is arranged to provide a purging fluid to the reactor. The purging fluid is provided at a temperature sufficient to provide cooling to the interior of the reactor and provided to purge the void of the reaction chamber 8 and the expansion space 9 of reaction byproducts. The reaction byproducts to be purged may include, but are not limited to, hydrogen gas, oxygen gas, and / or oxides of the molecules or ions. The purging fluid is preferably a liquid, such as water or an aqueous or non-aqueous electrolyte, which can be used to purge the void of the reaction chamber 8 and the expansion space 9 of electrolyte and / or byproducts that have been produced in the reaction chamber 8 or has entered the expansion space 9 from the reaction chamber 8 by passing through the anode plate 10 and the further separator 11. Use of the purging conduit 16 is not limited to the third embodiment and may be implemented in other embodiments of the invention, such as in the first and / or second embodiment(s).

[0084] In preferred embodiments, the at least one purging conduit 16 is provided in or as a part of the first back member 3a, such as the purging conduit being provided as one or more through-holes in the first back member 3a, within one or more through-holes of the first back member 3a and / or as one or more tubular protrusions on the first back member 3a.

[0085] In preferred embodiments the at least one purging conduit 16 is fluid ically connected to said expansion space 9 such that purging fluid used for purging the void of the reaction chamber 8 and the expansion space 9 of the byproducts flows 83369PC01

[0086] 15 through the at least one purging conduit 16 into the expansion space 9, through the further separator 11, the anode plate 10 and then enters the void of the reaction chamber 8, and then flows through the anode plate 10, the further separator 11 and the expansion space 9 before exiting the reactor through the at least one purging conduit.

[0087] In preferred embodiments the purging conduit 16 preferably comprises a purge inlet 16a and a purge outlet 16b both arranged in, such as through or being a part of, the first back member 3a. Purging fluid preferably flows from the purge inlet 16a into the expansion space 9 and exits through the purge outlet 16b. In another aspect of the embodiment the purge fluid flows from the purge outlet 16b into the expansion space 9 and exits through the purge inlet. In the embodiment illustrated in Fig. 2, the purge inlet and outlet 16a, 16b are provided by connecting pipes.

[0088] In preferred embodiments, the flow of electrolyte between the electrolyte inlet la and the electrolyte outlet lb and the flow of purging fluid between the purge inlet 16a and the purge outlet 16b both contribute to removing the byproducts of the graphite intercalation process from the void of the reaction chamber 8 and / or the expansion space 9 by transporting the reaction byproducts with the flow of the electrolyte and the purging fluid.

[0089] In the third embodiment, a set of gaskets are provided to create seals between adjoining surfaces between adjoining surfaces of the reactor in need of sealing to avoid leakage of electrolyte, purging fluid and / or graphite material to prevent electrolyte, purging fluid and / or graphite material from exiting the reaction chamber 8 or the expansion space 9 by passing between adjoining surfaces. Preferably, a first gasket 4a is provided between the first back member 3a and the expansion space wall elements 83, a second gasket 4b is provided between the expansion space wall elements 83 and the reaction chamber wall elements 82, and a third gasket 4c is provided between the reaction chamber wall elements 82 and the second back member 3b. The set of gaskets are preferably made from a resilient material, such as a rubber or a silicone. 83369PC01

[0090] 16

[0091] In preferred embodiments, a voltage source is provided to supply a difference in electrical potential between the cathode plate 6 and the anode plate 10. The difference in electrical potential of the cathode plate 6 and the anode plate 10 results in an electric field between the cathode plate inward surface 6b and the anode plate inward surface 10b which provides energy for driving the molecules or ions in the electrolyte into positions between graphene layers in the graphite material held in the void of the reaction chamber 8.

[0092] In preferred embodiments, the voltage source is provided as an external voltage source arranged exterior to, such as on an exterior of or at a distance from, said reactor and electrically connected to the anode plate 10 and the cathode plate 6. The voltage source can be one of, but is not limited to, an electric battery or a voltage source connected to an electrical grid.

[0093] In preferred embodiments all surfaces of the cathode plate 6 except for its inward surface 6b and / or all surfaces of the anode plate 10 except for its inward surface 10b may be electrically isolated from adjacent parts of the reactor in order to avoid short circuiting within the reactor when a voltage is applied between the cathode plate 6 and the anode plate 10 by the voltage source.

[0094] ITEMIZED LIST OF PREFERRED EMBODIMENTS

[0095] Item 1. A reactor for intercalating a graphite material, comprising

[0096] • an expandable reaction chamber (8) configured to retain an amount of graphite material and to allow for expansion of said graphite material during intercalation, wherein said expandable reaction chamber (8) being a first void interior of said reactor, said void being defined at least by:

[0097] - a fluid permeable cathode plate (6) comprising a cathode outward surface (6a) and a cathode inward surface (6b), said cathode inward surface (6b) facing said first void,

[0098] - a fluid permeable separator (7) arranged between said cathode inward surface (6b) and said graphite material,

[0099] - a fluid permeable anode plate (10) comprising an anode outward surface (10a) and an anode inward surface (10b), said anode inward surface (10b) facing said first void, 83369PC01

[0100] 17

[0101] - one or more wall elements (81) arranged to provide said void in combination with said cathode plate (6) and said anode plate (10),

[0102] - wherein said cathode plate (6) with said fluid permeable separator (7) and / or said anode plate (10) is / are moveably arranged so that an expansion of said expandable chamber (8) is provided by movement of said cathode plate (6) and / or said anode plate (10),

[0103] • a biasing member (13) for biasing said cathode plate (6) and / or said anode plate (10) towards said void by providing a force against said cathode plate outward surface (6a) and / or said anode plate outward surface (10a) in the direction of said void,

[0104] • a first back member (3a) arranged opposite said cathode plate outward surface (6a) or anode plate outward surface (10a) for providing an opposing force to said biasing member (13),

[0105] • at least one electrolyte supplying conduit (1) arranged to supply an electrolyte fluid to said void from an exterior of said reactor, said electrolyte supplying conduit (1) comprising at least one electrolyte inlet (la) and at least one electrolyte outlet (lb).

[0106] Item 2. A reactor according to item 1, wherein said expandable reaction chamber (8) is configured to expand in at least one direction perpendicular to a plane of said cathode plate (6) or said anode plate (10) by movement of said cathode plate

[0107] (6) and / or anode plate (10) in said direction.

[0108] Item 3. A reactor according to items 1 or 2, wherein said separator (7) is arranged to cover at least partly said cathode inward surface (6b).

[0109] Item 4. A reactor according to any one of the preceding items, further comprising an expansion space (9) configured for allowing expansion of said first void of the reaction chamber (8) by movement of said cathode plate (6) with said separator

[0110] (7) and / or said anode plate (10) at least partially into the expansion space (9).

[0111] Item 5. A reactor according to any one of the preceding items, wherein said reactor is in a stacked configuration, preferably with no externally moving parts. 83369PC01

[0112] 18

[0113] Item 6. A reactor according to any one of the preceding items, wherein said cathode plate (6), said anode plate (10), said expansion space (9), said biasing member (13), said first back member (3a) and said wall elements (81) are retained together in a stacked configuration by a locking arrangement.

[0114] Item 7. A reactor according to item 6, wherein said clamping arrangement comprises:

[0115] • at least two clamping members (2) arranged on opposite sides of said stacked configuration, and

[0116] • at least one clamping device for releasably clamping said at least two clamping members (2) against opposite sides of said stacked configuration.

[0117] Item 8. A reactor according to any one of the preceding items, wherein said biasing member (13) comprises at least one compression spring.

[0118] Item 9. A reactor according to any one of the preceding items, wherein said biasing member (13) comprises at least one pneumatic spring

[0119] Item 10. A reactor according to any one of the preceding items, wherein said reactor comprises a further separator (11) arranged between said biasing member (13) and said cathode outward surface (6a) or said anode outward surface (10a), said further separator (11) arranged to cover at least partly said cathode outward surface (6a) or said anode outward surface (10a).

[0120] Item 11. A reactor according to item 10, wherein said further separator (11) is fluid permeable.

[0121] Item 12. A reactor according to any one of the preceding items, where said electrolyte supplying conduit (1) comprises:

[0122] • a fluid distribution element (5) arranged in contact with the cathode outward surface (6a), wherein said fluid distribution element (5) is configured to distribute said electrolyte fluid flowing into said fluid distribution element (5) along the cathode outward surface (6a), wherein said fluid distribution element is fluidically connected to or forms part of said electrolyte supplying conduit (!)■ 83369PC01

[0123] 19

[0124] Item 13. A reactor according to any one of the preceding items, comprising a second back member (3b) through which a part of said electrolyte supplying conduit (1) extends.

[0125] Item 14. A reactor according to any one of the preceding items, wherein said at least one electrolyte inlet (la) and at least one electrolyte outlet (lb) both arranged exterior to said reactor.

[0126] Item 15. A reactor according to any one of the preceding items, comprising at least one purging conduit (16) arranged to supply a purge fluid to said expansion space (9) and said cathode outward surface (6a) or said anode cathode outward surface (10a), or when dependant on item 7, a surface of said further separator (11), said purging conduit (16) comprises at least one purge inlet (16a) and at least one purge outlet (16b) arranged to allow purge fluid to flow to an exterior of said reactor, said purge inlet (16a) and purge outlet (16b) are preferably arranged exterior to said reactor.

[0127] Item 16. A reactor according to item 15, wherein said first back member (3a) comprises at least one through-hole forming part of said purging conduit (16).

[0128] Item 17. A reactor according to any one of items 15 or 16, when dependant on item 3, wherein said at least one purging conduit (16) is fluidica lly connected to said expansion space (9).

[0129] Item 18. A reactor according to any one of items 15-17, wherein said purging conduit (16) comprises a purge inlet (16a) and a purge outlet (16b) both arranged exterior to said reactor.

[0130] Item 19. A reactor according to any one of the preceding items, wherein said wall elements (81) comprise:

[0131] • reaction chamber wall elements (82), arranged adjacently to said second back member (3b), wherein said reaction chamber wall elements (82) are arranged to at least partially surround said expandable reaction chamber (8), and 83369PC01

[0132] 20

[0133] • expansion space wall elements (83), arranged between said reaction chamber wall elements (82) and said first back member (3a), wherein said expansion space wall elements (83) are arranged to at least partially surround said expansion space (9), wherein said reaction chamber wall elements (82) and said expansion space wall elements (83) are arranged to maintain a predetermined spatial orientation of said cathode plate (6) with said separator (7) or said anode plate (10) relative to said reaction chamber wall elements (82) and said expansion space wall elements (83) during movement of said cathode plate (6) with said separator (7) or said anode plate (10).

[0134] Item 20. A reactor according to item 19, further comprising a set of gaskets (4a, 4b, 4c), wherein a first gasket (4a) is provided between said first back member (3a) and said expansion space wall elements (83), and / or wherein a second gasket (4b) is provided between said expansion space wall elements (83) and said reaction chamber wall elements (82), and / or wherein a third gasket (4c) is provided between said reaction chamber wall elements (82) and said second back member (3b).

[0135] Item 21. A reactor according to any one of the preceding items, wherein a voltage source is electrically connected to said cathode plate (6) and said anode plate (10), the voltage source is arranged to provide a difference in electrical potential between said cathode plate (6) and said anode plate (10).

[0136] LIST OF REFERENCE SYMBOLS USED

[0137] 1 Electrolyte supplying conduit la Electrolyte inlet lb Electrolyte outlet

[0138] 2 Clamping member

[0139] 3a First back member

[0140] 3b Second back member

[0141] 4 Gasket

[0142] 4a First gasket

[0143] 4b Second gasket

[0144] 4c Third gasket 83369PC01

[0145] 21

[0146] 5 Fluid distribution element

[0147] 6 Fluid permeable cathode plate

[0148] 6a Cathode plate outward surface

[0149] 6b Cathode plate inward surface

[0150] 7 Fluid permeable separator

[0151] 8 Reaction chamber

[0152] 9 Expansion space

[0153] 10 Fluid permeable anode plate

[0154] 10a Anode plate outward surface

[0155] 10b Anode plate inward surface

[0156] 11 Further separator

[0157] 13 Biasing member

[0158] 13a Compression spring

[0159] 16 Purging conduit

[0160] 16a Purge inlet

[0161] 16B Purge outlet

[0162] 81 Wall elements

[0163] 82 Reaction chamber wall elements

[0164] 83 Expansion space wall elements

[0165] Although the present invention has been described in connection with the specified embodiments, it should not be construed as being in any way limited to the presented examples. The scope of the present invention is set out by the accompanying claim set. In the context of the claims, the terms "comprising" or "comprises" do not exclude other possible elements or steps. Also, the mentioning of references such as "a" or "an" etc. should not be construed as excluding a plurality. The use of reference signs in the claims with respect to elements indicated in the figures shall also not be construed as limiting the scope of the invention. Furthermore, individual features mentioned in different claims, may possibly be advantageously combined, and the mentioning of these features in different claims does not exclude that a combination of features is not possible and advantageous.

Claims

83369PC0122CLAIMS1. A reactor for intercalating a graphite material, comprising• an expandable reaction chamber (8) configured to retain an amount of graphite material and to allow for expansion of said graphite material during intercalation, wherein said expandable reaction chamber (8) being a first void interior of said reactor, said void being defined at least by:- a fluid permeable cathode plate (6) comprising a cathode outward surface (6a) and a cathode inward surface (6b), said cathode inward surface (6b) facing said first void,- a fluid permeable separator (7) arranged between said cathode inward surface (6b) and said graphite material,- a fluid permeable anode plate (10) comprising an anode outward surface (10a) and an anode inward surface (10b), said anode inward surface (10b) facing said first void,- one or more wall elements (81) arranged to provide said void in combination with said cathode plate (6) and said anode plate (10),- wherein said cathode plate (6) with said fluid permeable separator (7) and / or said anode plate (10) is / are moveably arranged so that an expansion of said expandable chamber (8) is provided by movement of said cathode plate (6) and / or said anode plate (10),• a biasing member (13) for biasing said cathode plate (6) and / or said anode plate (10) towards said void by providing a force against said cathode plate outward surface (6a) and / or said anode plate outward surface (10a) in the direction of said void,• a first back member (3a) arranged opposite said cathode plate outward surface (6a) or anode plate outward surface (10a) for providing an opposing force to said biasing member (13),• at least one electrolyte supplying conduit (1) arranged to supply an electrolyte fluid to said void from an exterior of said reactor, said electrolyte supplying conduit (1) comprising at least one electrolyte inlet (la) and at least one electrolyte outlet (lb).

2. A reactor according to claim 1, wherein said expandable reaction chamber (8) is configured to expand in at least one direction perpendicular to a plane of said83369PC0123 cathode plate (6) or said anode plate (10) by movement of said cathode plate (6) and / or anode plate (10) in said direction.

3. A reactor according to claim 1 or 2, wherein said separator (7) is arranged to cover at least partly said cathode inward surface (6b).

4. A reactor according to any one of the preceding claims, further comprising an expansion space (9) configured for allowing expansion of said first void of the reaction chamber (8) by movement of said cathode plate (6) with said separator (7) and / or said anode plate (10) at least partially into the expansion space (9).

5. A reactor according to any one of the preceding claims, wherein said reactor is in a stacked configuration, preferably with no externally moving parts.

6. A reactor according to any one of the preceding claims, wherein said cathode plate (6), said anode plate (10), said expansion space (9), said biasing member (13), said first back member (3a) and said wall elements (81) are retained together in a stacked configuration by a clamping arrangement.

7. A reactor according to claim 6, wherein said clamping arrangement comprises:• at least two clamping members (2) arranged on opposite sides of said stacked configuration, and• at least one clamping device for releasably clamping said at least two clamping members (2) against opposite sides of said stacked configuration.

8. A reactor according to any one of the preceding claims, wherein said biasing member (13) comprises at least one compression spring.

9. A reactor according to any one of the preceding claims, wherein said biasing member (13) comprises at least one pneumatic spring.

10. A reactor according to any one of the preceding claims, wherein said reactor comprises a further separator (11) arranged between said biasing member (13) and said cathode outward surface (6a) or said anode outward surface (10a), said83369PC0124 further separator (11) arranged to cover at least partly said cathode outward surface (6a) or said anode outward surface (10a).

11. A reactor according to claim 10, wherein said further separator (11) is fluid permeable.

12. A reactor according to any one of the preceding claims, where said electrolyte supplying conduit (1) comprises:• a fluid distribution element (5) arranged in contact with the cathode outward surface (6a), wherein said fluid distribution element (5) is configured to distribute said electrolyte fluid flowing into said fluid distribution element (5) along the cathode outward surface (6a), wherein said fluid distribution element is fluidically connected to or forms part of said electrolyte supplying conduit (1).

13. A reactor according to any one of the preceding claims, comprising a second back member (3b) through which a part of said electrolyte supplying conduit (1) extends.

14. A reactor according to any one of the preceding claims, wherein said at least one electrolyte inlet (la) and at least one electrolyte outlet (lb) both arranged exterior to said reactor.

15. A reactor according to any one of the preceding claims, comprising at least one purging conduit (16) arranged to supply a purge fluid to said expansion space (9) and said cathode outward surface (6a) or said anode cathode outward surface (10a), or when dependant on claim 7, a surface of said further separator (11), said purging conduit (16) comprises at least one purge inlet (16a) and at least one purge outlet (16b) arranged to allow purge fluid to flow to an exterior of said reactor, said purge inlet (16a) and purge outlet (16b) are preferably arranged exterior to said reactor.

16. A reactor according to claim 15, wherein said first back member (3a) comprises at least one through-hole forming part of said purging conduit (16).83369PC012517. A reactor according to any one of claims 15 or 16, when dependant on claim 3, wherein said at least one purging conduit (16) is fluidica lly connected to said expansion space (9).

18. A reactor according to any one of claims 15-17, wherein said purging conduit (16) comprises a purge inlet (16a) and a purge outlet (16b) both arranged exterior to said reactor.

19. A reactor according to any one of the preceding claims, wherein said wall elements (81) comprise:• reaction chamber wall elements (82), arranged adjacently to said second back member (3b), wherein said reaction chamber wall elements (82) are arranged to at least partially surround said expandable reaction chamber (8), and• expansion space wall elements (83), arranged between said reaction chamber wall elements (82) and said first back member (3a), wherein said expansion space wall elements (83) are arranged to at least partially surround said expansion space (9), wherein said reaction chamber wall elements (82) and said expansion space wall elements (83) are arranged to maintain a predetermined spatial orientation of said cathode plate (6) with said separator (7) or said anode plate (10) relative to said reaction chamber wall elements (82) and said expansion space wall elements (83) during movement of said cathode plate (6) with said separator (7) or said anode plate (10).

20. A reactor according to claim 19, further comprising a set of gaskets (4a, 4b, 4c), wherein a first gasket (4a) is provided between said first back member (3a) and said expansion space wall elements (83), and / or wherein a second gasket (4b) is provided between said expansion space wall elements (83) and said reaction chamber wall elements (82), and / or wherein a third gasket (4c) is provided between said reaction chamber wall elements (82) and said second back member (3b).

21. A reactor according to any one of the preceding claims, wherein a voltage source is electrically connected to said cathode plate (6) and said anode plate83369PC0126(10), the voltage source is arranged to provide a difference in electrical potential between said cathode plate (6) and said anode plate (10).

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