Classifications

• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/04—Construction or manufacture in general
  • H01M10/0413—Large-sized flat cells or batteries for motive or stationary systems with plate-like electrodes
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M4/00—Electrodes
  • H01M4/02—Electrodes composed of, or comprising, active material
  • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/05—Accumulators with non-aqueous electrolyte
  • H01M10/052—Li-accumulators
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/05—Accumulators with non-aqueous electrolyte
  • H01M10/052—Li-accumulators
  • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M10/00—Secondary cells; Manufacture thereof
  • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
  • H01M10/4214—Arrangements for moving electrodes or electrolyte
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M4/00—Electrodes
  • H01M4/02—Electrodes composed of, or comprising, active material
  • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
  • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
  • H01M50/60—Arrangements or processes for filling or topping-up with liquids; Arrangements or processes for draining liquids from casings
  • H01M50/691—Arrangements or processes for draining liquids from casings; Cleaning battery or cell casings
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
  • H01M50/70—Arrangements for stirring or circulating the electrolyte
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
  • H01M2200/00—Safety devices for primary or secondary batteries
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
  • Y02E60/10—Energy storage using batteries
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
  • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

• the invention relates to the arrangement of a lithium accumulator comprising a stack of electrodes which are detachable from one another in the event of an emergency situation (short circuit, overheating, mechanical damage), and additionally the space between the electrodes is flooded by an emergency liquid, which displaces the electrolyte and stops ion transfer between the electrodes.
• the inactivation of the accumulator is fully reversible: after the emergency situation has elapsed, the accumulator can be easily and quickly put into its original operating state.
• the arrangement of the accumulator according to the invention can provide high capacity, for example using an electrode made of metal lithium, while ensuring high safety of the accumulator operation.
• the current standard solution is the use of an electronic security circuit that includes a temperature sensor and which disconnects the accumulator when the accumulator temperature limits are exceeded.
• the document WO2005324563 solves the problem partially by accumulator groups being stored in a substrate which makes the accumulator system vibration-resistant and the system is interposed by tubes through which the heat exchange medium flows.
• the document WO20010031363 discloses a lithium accumulator consisting of a stack of superposed metal frames in which thick-walled electrodes are disposed, the opposite polarity electrodes being separated by separators and the opposing polarity frames being isolated from each other.
• metal frames allow for better heat removal from the interior of the accumulator, they do not guarantee the heat removal to the required extent.
• the document WO2012038887 discloses another solution for regulating the temperature of a high-capacity lithium accumulator by using a liquid electrolyte which also serves as a cooling medium.
• the Czech Patent No. 306913 solves the problem by providing an accumulator structure consisting of mutually detachable electrode modules, wherein in an emergency situation not only the electrode modules are detached, but the negative electrode module is flooded with the emergency medium.
• the above mentioned solutions are relatively demanding in respect to the arrangement of the accumulator, and moreover, they do not allow immediate and complete inactivation of the accumulator electrodes.
• Such an accumulator can reach several fold higher capacity, while reducing weight and size compared to current standard accumulators.
• the objective is to have the electrodes immediately and fully inactivated under emergency situation, so that the accumulator could not inflame or explode.
• Such a lithium accumulator arrangement would meet the highest safety requirements even under extreme conditions and accidents.
• the accumulator arrangement according to the invention allows to use preferably metal lithium (Li), or lithium in dendritic form, for negative electrode, in combination with a positive electrode of vanadium oxide (V 2 O 5 ) or Li-NMC (Li(NiMnCo)0 2 ) to achieve extremely high capacity.
• the arrangement of the accumulator according to the invention can of course be used for electrodes formed by standard lithium compounds, e.g. lithium salts, known in the art.
• the simultaneous detaching of the electrodes and the flooding of the electrodes by the emergency liquid prevents ion transfer in the interspaces between the electrodes and thus stops the increase of the temperature of the accumulator.
• the electrolyte flashing temperature is significantly increased from common 140 °C - 170 °C (for standard electrolytes comprising Li salts in a non-aqueous organic solvent) to 230 °C or more.
• the present invention provides an accumulator comprising an electrode module enclosed in the outer solid casing, whereas the module comprises an electrolyte and a stack of plate electrodes clamped between the lower and upper lid and the upper lid is releasable (which means it can be released and shifted or displaced).
• the electrode stack comprises at least one negative electrode and at least one positive electrode and at least one separator.
• the individual electrodes are detachable (which means they can be shifted or mutually moved away) from one another after releasing the upper lid.
• the electrode module is equipped with at least one tube for supplying the emergency liquid into the space between the electrodes.
• the electrodes are shiftably (slidably) mounted on at least one supporting plug so that the electrodes can be moved in the direction of the longitudinal axis of the plug.
• the electrode stack preferably comprises a plurality of electrodes, e.g., 6, 8, 12, 24, of the electrodes of each polarity.
• the supporting plug is located substantially perpendicular to the lower and upper lids, passes through the opening in the electrodes, particularly in the electrode frame, or optionally through the upper lid, or the lower lid as the case may be.
• the individual electrodes are therefore mechanically detachable from each other after releasing the upper lid by the action of an elastic member located between the electrodes.
• the elastic member can be, for example, a spring, preferably made of a non-conductive material, or an elastic block, e.g. a rubber block. In another embodiment, the elastic member may simultaneously perform the function of an elastic or extendable conductive junction of the electrodes.
• the upper lid and the electrodes can be returned to the original clamped position easily after overcoming the force of the elastic members between the electrodes.
• two supporting plugs are used which can simultaneously perform the function of the current collector and the poles of the accumulator, whereas the electrodes of one polarity are mounted on the first plug and the electrodes of the other polarity are mounted on the second plug.
• the electrode stack contains negative and positive electrodes, usually arranged alternately, and separated by separators.
• the top and bottom lids are separated from the electrodes by an insulator.
• the upper lid and the electrodes are penetrated by at least one tube for injecting the emergency liquid into the inner space of the electrode module.
• the lower and upper lids are clamped by at least one clamping member, preferably a bolt, which passes through the lid and is provided with a safety lock that secures the position of the upper releasable lid and, if necessary, enables it to be released.
• the clamping member extends outside the electrode frames. Preferably, four clamping bolts are used. Electrodes of the same type are connected to each other by flexible or extendable conductive junctions and are also connected to the respective pole of the accumulator.
• the electrode module is preferably provided with a stretchable (i.e.
• expandable and back-shrinkable) container which is made, for example, from a laminated plastic film which is commonly known to the person skilled in the art and which is impermeable to the electrolyte.
• This stretchable container is thus filled with electrolyte and isolates the electrode stack or the entire electrode module from the outer solid casing of the accumulator.
• the space between the outer solid casing and the stretchable container is preferably filled with an inert gas during the operation of the accumulator which protects the metal lithium inside the accumulator.
• the stretchable container in its expanded state i.e.
• Double accumulator packaging also contributes to increased safety of the operation of the accumulator.
• the electrode comprises a conductive frame, preferably provided with a contact nose, in which the opening for slipping the frame on the supporting plug is preferably located.
• the frame In the frame, at least one opening for insertion of the emergency liquid supply tube is formed.
• the frame is in the shape of an annulus which is provided with two openings for inserting the emergency liquid supply tube.
• the tubes may be used for filling the accumulator with an electrolyte, whereby preferably one tube is used for filling and at least one other tube is used for de-aeration.
• the electrodes are equipped with a cap gasket on their circumference, which covers the entire frame on both sides and serves for electrical isolation of the electrodes. The cap gasket is provided with a lateral opening allowing the contact nose to protrude outside.
• the bottom of the electrode is connected, preferably by pressing or welding, from the lower side of the frame.
• the bottom is formed from the conductive, electrolyte permeable material, e.g. expanded metal, grid, net or perforated foil, preferably expanded metal. Any other layers with an area substantially identical to the inside area of the frame may be inserted and pressed from above.
• the active material of the electrode is deposited, preferably pressed, from above, so as to form a layer that preferably does not exceed the upper edge of the frame.
• the negative electrode frame is preferably made of copper (Cu), the bottom is preferably made of Cu or Li, preferably in the form of an expanded metal, and the active material of the negative electrode is metal Li, preferably in the form of metal sheet, grid, or dendrites.
• the positive electrode has a frame preferably made from aluminium (Al), the bottom is preferably also made of Al, preferably in the form of an expanded metal, and the active material is vanadium oxide or NMC (Li(NiMnCo)0 2 ), preferably vanadium pentoxide (V 2 O 5 ).
• the material of the separators may by porous film made of nonwoven glass or ceramic fibres which are known to a person skilled in the art and are commercially available.
• the electrolyte for the accumulator according to the invention is one of the conventional electrolyte type of non-aqueous organic solvent + Li salts known to a person skilled in the art.
• the emergency liquid supply tube is made of a non-conductive material, preferably ceramic or plastic.
• the tube is inserted into the electrode stack from above to the bottom, i.e. to the lower lid.
• the tube is adapted to cause the emergency fluid to easily penetrate into the space between the electrodes throughout its active length (i.e. part inserted into the electrode stack).
• the tube is perforated.
• the passage of the tube through the upper lid and the outer solid accumulator casing is sealed in a suitable manner.
• the safe operation of the accumulator according to the present invention is ensured by the arrangement that allows, under emergency situation, releasing the safety lock(s) on the clamping bolt(s) and detaching the electrodes by the effect of the elastic members between the electrodes, and simultaneously filling the spaces between the electrodes by the emergency liquid.
• the safety lock on the clamping bolt can, for example, be in the form of a safety pin or ring which, in the event of an emergency, is released by an electromagnetic or hydraulic system. Safety locks of such a type are commonly known to those skilled in the art.
• a safety container filled with the emergency liquid which is preferably mineral oil, and pressurized inert gas, preferably argon, which serves to expel the emergency fluid, is connected to the emergency liquid supply tube via a safety valve.
• the safety container may be in the form of a separate structure member, or it may be suitably integrated with the accumulator and be, for example, a part of the outer casing of the accumulator. Similar solutions are known to those skilled in the art.
• the temperature and shock monitoring system is a part of the emergency accumulator system, which is equipped with sensors that, when the set limits are exceeded, activate the emergency mode, disconnect the electrical circuit and open the safety lock(s) and open/close the respective valves.
• This part of the emergency system is not described in more detail here since it belongs to common parts of the lithium accumulator safety systems and it is known to those skilled in the art.
• safety locks on the clamping bolts are open, the upper lid is released and by the effect of the elastic elements between the electrodes, the electrodes will be practically immediately detached, while simultaneously the emergency liquid is injected (by means of pressurized argon) into the spaces between the electrodes.
• Emergency fluid impregnates the separators and displaces the electrolyte into the space outside the electrodes (from where it can escape through the safety valve), preferably into the space defined by the stretchable container within the outer solid casing.
• Emergency liquid fills the space between the electrodes, saturates the lithium surfaces, interrupts the transfer of ions between the electrodes and also cools the accumulator to prevent unwanted chemical reaction of lithium. This eliminates the cause of eventual fire or explosion of the accumulator.
• the above-described emergency accumulator inactivation is fully reversible. After the emergency situation has elapsed, the electrodes can be easily returned from the expanded position to the original operating position (clamped), the emergency liquid displaced and replaced again with the electrolyte.
• the new accumulator arrangement allows the use of metal lithium for the negative electrode.
• the theoretical capacity increase using metal lithium over lithium salts is up to twenty times. And the accumulator safety is maintained or even increased.
• the accumulators of the invention can be used as single cells and assembled into batteries containing, for example, 3, 6 or 12 cells, by the way described for example in utility model No. CZ 30997, or by any other way known to a person skilled in the art.
• Metal lithium electrodes combined with vanadium oxide electrodes mean also that expensive metals like nickel, cobalt and molybdenum are not needed for the manufacturing of electrodes. Further advantage is that the assembly of such an accumulator can be carried out under normal ambient atmosphere. Before filling in the electrolyte, however, the inner space of the electrode module is preferably blown through by the dried air.
• the subject-matter of the present invention is a high-capacity lithium accumulator with increased operational safety as described above and as defined in the appended patent claims.
• a further subject-matter of the invention is a method of safely operating a lithium accumulator as described above and as defined in the appended patent claims.
• FIG. 1 A scheme of the accumulator - sectional view. Hatched arrows indicate the direction of the upper lid release and the shift of the electrodes when they are detached.
• Fig. 2. A schematic view of the accumulator A) from the top lid side and B) from the lower lid side.
• FIG. 3 A scheme A) of the clamping bolts with the safety lock and B) and the supporting plug provided with the contact for the accumulator pole.
• Fig. 4 A schematic representation of A) the negative electrode frame and B) the positive electrode frame.
• FIG. 5 A schematic representation of A) ring cap gasket (in bottom part of the figure is a scheme of cross section of the gasket) and B) the separator.
• Fig. 6 A schematic representation of A) the negative electrode bottom placement in respect to the electrode frame and B) the negative electrode material applied to the bottom connected to the frame.
• the scheme may apply analogously to the positive electrode.
• FIG. 7 A scheme of a preferred embodiment of the accumulator - sectional view.
• the arrows indicate the direction of the upper lid release and the shift of the electrodes when they are detached.
• FIG. 1 A schematic diagram illustrating the basic principle of the arrangement of the accumulator according to the invention is shown in cross-section in Fig. 1.
• Fig. 7 another preferred embodiment of the accumulator is shown in the same cross-section view.
• Figures 2 to 6 show details of selected components of the accumulator, which will be described in more detail below.
• the accumulator comprises the electrode module that is encased in the solid casing I .
• the electrode module comprises a stack of plate electrodes 2, 3 in which the negative electrodes 2 and positive electrodes 3 are alternated, the stack being pressed and clamped between the lower lid 4 and the releasable upper lid 5.
• the electrodes 2, 3 are slidably mounted on the two supporting plugs 6, 7 so that the electrodes 2, 3 can be shifted in the direction of the longitudinal axis of the supporting plugs 6, 7 and moved away from each other.
• the supporting plugs 6, 7 are oriented perpendicularly to the lower lid 4 (and to the upper lid 5 as well) and they form simultaneously the poles of the accumulator.
• the supporting plugs 6, 7 pass through the respective electrodes 2, 3 (through the opening in the contact nose 22, 32 of the frame 21, 3J_, as will be explained hereinafter) as well as through the opening or slot in the upper lid 5.
• the supporting plugs 6, 7 are secured by nuts 19 at their bottom end (below the lowest of the electrodes 2, 3).
• conductive springs 8 are provided, the function of which is to mechanically move away the electrodes 2, 3 after releasing the upper lid 5.
• the springs 8 also fulfil the function of the flexible or extendable conductive electrical junctions 81 which interconnect the respective electrodes 2, 3.
• the electrodes 2, 3 are separated by separators 9.
• the upper lid 5 and the lower lid 4 are isolated from the electrodes 2, 3 by the insulator 1_8.
• the lower lid 4 and the upper lid 5 are essentially a circular plate made of aluminium sheet 4 mm thick (the thickness of the plate will be adapted to the amount of stacked electrodes 2, 3) and with the diameter of 178 mm.
• the upper lid 5 is provided with openings for the passage of the clamping bolts 11 and the emergency liquid supplying tubes 10.
• the upper lid 5 is further provided with an opening or slot for the passage of the supporting plugs 6, 7.
• the lower lid 4 is provided with openings for the clamping bolts 11.
• Two emergency liquid supplying tubes 10 pass through the upper lid 5 and the electrodes 2, 3 in the region of the frame 21, 31 and extend to the lower lid 4.
• the lower lid 4 and the upper lid 5 are clamped by means of four clamping bolts 11 which are provided with a nut 12 on the lower end and by a safety lock 13 on the upper end.
• the outer diameter of the frame 21, 31 of the electrodes 2, 3 is smaller than the diameter of the lower lid 4 and of the upper lid 5 so that the openings for clamping bolts 11 are formed near the periphery of the lid 4, 5_outside the area in which the frames 21, 32 overlap with the lids 4, 5. This means that the clamping bolts 11 do not interfere with the inner space of the electrodes 2, 3.
• Each electrode 2, 3 comprises an annular frame 21, 31 which is provided with two openings for inserting an emergency liquid supply tube 10.
• Each electrode 2, 3 has a semicircular contact nose 22, 32. These contact noses 22, 32 are oriented oppositely when assembling the stack of electrodes 2, 3.
• the frame 21, 31 is slidably mounted on the supporting plugs 6, 7 by the opening in the contact nose 22, 32.
• the conductive bottom 23, 33 formed of expanded metal is pressed onto the frame 21, 31 from the lower side.
• the active material 24, 34 is deposited in the bottom 23, 33 within the frame 21, 31 from the upper side.
• the frame 21 of the negative electrode 2 is made of copper (Cu) of 1 mm thickness
• the bottom 23 is made up of Li expanded metal.
• the active material 24 of the negative electrode 2 is Li metal.
• the positive electrode 3 has the frame 31 made of aluminium (Al) of 2 mm thickness, the bottom 33 is of Al expanded metal, and the active material 34 is V 2 O 5 .
• the outer diameter of the frame 21, 3J_ is 143 mm; the inner diameter is 113 mm.
• the diameter of the bottom 23, 33 is larger than the inner diameter of the frame 21, 3J_ and is smaller than its outer diameter, in this example it is 133 mm.
• the gasket 16 is provided with a lateral opening 17 which allows the contact nose 22, 32 to protrude outside.
• the separators 9 are porous films made of nonwoven glass or ceramic fibres conventionally used as separators in Li cells.
• the separators 9 are in the shape of a disc which has a diameter substantially equal to the outer diameter of the frame 21, 31, or slightly smaller, in particular in this example the diameter is 141 mm.
• the separators 9 are provided with openings for the passage of the emergency liquid supplying tubes 10.
• the electrode module is further provided with a stretchable container 14, which is made of an elastic plastic film, impermeable to the electrolyte.
• the space of the stack of the electrodes 2, 3 enclosed in the stretchable container 14 is filled with an electrolyte.
• the space between the stretchable container 14 and the solid casing 1 is filled with argon.
• the solid casing 1 is provided with a safety valve 15 for expelling argon.
• the emergency liquid supply tubes 10 are made of ceramic and their parts inserted into the stack of electrodes 2, 3 are perforated to allow rapid penetration of the emergency liquid into the spaces between the electrodes 2, 3.
• the supporting plugs 6, 7 are provided with pole extensions which pass, as well as the emergency liquid supply tubes 10, through the upper part of the solid casing 1.
• the electrodes 2, 3 of the same polarity are electrically interconnected with extendable electric junctions 8 and elastic rubber blocks 81 are inserted between the electrodes 2, 3, whereas the function of the blocks 81 is to move the electrodes 2, 3 away after the upper lid 5 has been released.
• the stretchable container 14 is positioned so as to only cover the stack of the electrodes 2, 3 including the separators 9, between the lower lid 4 and the upper lid 5.
• the positive electrodes 3 are doubled (there is a larger amount of active material 34 of the positive electrode 3 to achieve higher power).
• the present invention allows the use of metal lithium in accumulators to approximate the real voltage and accumulator capacity to the maximum theoretical values and thus to achieve a significant increase of the capacity/weight ratio for the accumulator.
• the invention can be used for manufacturing high-capacity accumulators with enhanced safety which will be useful especially where high capacity, low weight and high safety are required, particularly in vehicles such as automobiles or ships.
• the metal lithium accumulator with a theoretical capacity of 3880 mAh/g of metal lithium, compared to a capacity of 175 mAh/g of lithium salts, can achieve theoretically 20times the capacity at the same weight of the negative electrode material.

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Citations (7)

• 2017
  • 2017-10-13 CZ CZ2017-656A patent/CZ2017656A3/cs unknown
  • 2017-11-02 WO PCT/CZ2017/050055 patent/WO2019072320A1/en not_active Ceased

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