Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
  • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
  • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
  • B01J20/2805—Sorbents inside a permeable or porous casing, e.g. inside a container, bag or membrane
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
  • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
  • B01D53/0407—Constructional details of adsorbing systems
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
  • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/26—Drying gases or vapours
  • B01D53/261—Drying gases or vapours by adsorption
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/34—Chemical or biological purification of waste gases
  • B01D53/46—Removing components of defined structure
  • B01D53/62—Carbon oxides
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
  • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
  • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
  • B01J20/041—Oxides or hydroxides
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
  • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
  • H01G11/04—Hybrid capacitors
  • H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
• • 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
  • H01M10/52—Removing gases inside the secondary cell, e.g. by absorption
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2251/00—Reactants
  • B01D2251/30—Alkali metal compounds
  • B01D2251/302—Alkali metal compounds of lithium
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2251/00—Reactants
  • B01D2251/40—Alkaline earth metal or magnesium compounds
  • B01D2251/402—Alkaline earth metal or magnesium compounds of magnesium
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2251/00—Reactants
  • B01D2251/40—Alkaline earth metal or magnesium compounds
  • B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2251/00—Reactants
  • B01D2251/60—Inorganic bases or salts
  • B01D2251/602—Oxides
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2251/00—Reactants
  • B01D2251/60—Inorganic bases or salts
  • B01D2251/604—Hydroxides
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/106—Silica or silicates
  • B01D2253/108—Zeolites
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
  • B01D2253/1124—Metal oxides
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/30—Physical properties of adsorbents
  • B01D2253/302—Dimensions
  • B01D2253/304—Linear dimensions, e.g. particle shape, diameter
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2257/00—Components to be removed
  • B01D2257/50—Carbon oxides
  • B01D2257/504—Carbon dioxide
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2257/00—Components to be removed
  • B01D2257/80—Water
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/414—Further details for adsorption processes and devices using different types of adsorbents
  • B01D2259/4141—Further details for adsorption processes and devices using different types of adsorbents within a single bed
  • B01D2259/4143—Further details for adsorption processes and devices using different types of adsorbents within a single bed arranged as a mixture
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/26—Drying gases or vapours
  • B01D53/28—Selection of materials for use as drying agents
• • 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
• • 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
  • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
  • Y02C20/00—Capture or disposal of greenhouse gases
  • Y02C20/40—Capture or disposal of greenhouse gases of CO2
• • 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

Definitions

• the present invention in a first aspect thereof is inherent to an improved carbon dioxide composite getter and in a second aspect thereof to sealed systems employing such an improved carbon dioxide composite getter.
• Non-limiting examples of systems negatively affected by chemical interactions are organic electronic devices, while examples of the latter type of devices where is the physical interaction to determine a device deterioration, are typically the ones where C0 2 is produced by the systems themselves as a side effect of their operation, and this may lead to overpressure and consequent rupture of the device case.
• Rechargeable lithium batteries are among the most critical devices since carbon dioxide overpressure may lead to sudden rupture of the device case with the risk of leakage of flammable substances (the electrolytes contained therein). This problem is also enhanced by the fact that typically the free volume in these devices is very small, whereby the generation of low quantities of carbon dioxide will lead to a quick rise in the device internal pressure.
• the purpose of the present invention is to provide an improved carbon dioxide composite getter comprising an envelope permeable to C0 2 defining an internal volume V, that contains powders of a first and a second active materials whose cumulative volume is Vm, characterized in that said first active material is lithium hydroxide and said second active material is lithium oxide, and the LiOH/Li 2 0 molar ratio is comprised between 0,05 and 1,5
• cumulative volume Vm it is meant the overall sum of the active materials (lithium oxide and lithium hydroxide) particles volume contained within the internal volume V defined by the C0 2 -permeable envelope.
• the molar ratio is preferably comprised between 0,05 and 0,2 for all those applications where the composite getter sorption speed is less important and that instead require higher C0 2 capacity, while a ratio comprised between 0,2 and 0,7 would provide a compromise solution between optimal C0 2 sorption speed and C0 2 removal capacity, and when the ratio is comprised between 0,7 and 1 ,5 the getter has its sorption speed optimized.
• C0 2 -permeable envelope a material that has a C0 2 permeation coefficient of at least 50 cm 3 *mm/(m 2 *day*atm), said value being preferably equal to or higher than 100.
• the C0 2 -permeable envelope preferably usefully exhibits a moisture vapor transmission rate (MVTR) that is not higher than 0,6 g*mm/(m 2 *day).
• MVTR moisture vapor transmission rate
• FIG. 2 shows a cross section view of a second embodiment of a C0 2 composite getter system according to the present invention
• Li 2 0 + H 2 0 ⁇ 2 ⁇ (I) Li 2 0 + H 2 0 ⁇ 2 ⁇ (I)
• the lithium hydroxide reacts with carbon dioxide according to the following reaction:
• the inventors have surprisingly and unexpectedly found that such combination of materials requires also additional conditions in order to be an effective CO2 getter; in particular the novel combination of active materials according to the present invention, i.e. lithium hydroxide combined with an excess of lithium oxide, shall be confined in a volume, smaller than the volume of the sealed device, by means of a C02-permeable envelope.
• Such volume, together with the characteristic and behavior of the CO2- permeable envelope provides the appropriate environment for CO2 capture (as per reaction II) and for the conversion of lithium oxide into lithium hydroxide (as per reaction I).
• the lithium hydroxide and lithium oxide powders are mixed together and put into a C0 2 -permeable "pouch" that is sealed, for example, by heating.
• the ratio of the active material volume Vm to the getter system internal volume V is comprised between 0,15 and 0,9.
• the C0 2 composite getter comprises a dispersion in a suitable polymeric binder of lithium hydroxide and lithium oxide in the correct ratio, as above defined, which is in contact with a C0 2 -permeable envelope, as per definition provided above.
• the C0 2 -permeable envelope although defining an internal volume V, does not completely surround the polymeric binder, i.e. a small portion of the binder containing the first and second active materials is not covered by the envelope.
• the binder defines the internal volume V. It is important that only a small fraction of the binder is not covered/coated with the C0 2 -permeable envelope, i.e.
• the internal volume in this case is equivalently and sufficiently defined both by the envelope covering at least 95% of the surface area of the binder and therefore defining an internal volume presenting a small aperture, as well as the binder with the active material powders that represents the internal volume.
• the level of loading of the powders into the polymeric binder assures the presence of an optimized "reaction volume" for the powders of the two active materials and in particular this condition is achieved when the overall loading level for the LiOH and Li 2 0 powders into the polymeric binder is comprised between 20 and 60 wt%, and preferably comprised between 40 and 50 wt%.
• the additional element for H 2 0 removal is actually a "precursor" for the C0 2 adsorber, resulting in a system having a higher capacity with respect to systems associating the lithium hydroxide with a generic moisture removing material.
• the structure of the getter system according to the present invention is one that while providing a suitable reaction volume renders the C0 2 sorption characteristics suitable to control the pressure within sealed devices, by providing a good capacity coupled with an appropriate reaction kinetics.
• FIG. 1 A cross-sectional view of a composite C0 2 getter system 10 according to the present invention is shown in Figure 1 , showing particles of lithium oxide 11, 11 ', 11 " (white circles), and of lithium hydroxide 12, 12', 12" (black circles), surrounded by a C0 2 permeable envelope 14.
• the system 10 presents an internal free volume 13 (indicated in white) .
• Lithium oxide particles and lithium hydroxide particles are represented as circles even though in reality and in the most common cases their shape is not regular. Also the getter system 10 has been depicted with a regular and rectangular shape, but any shape is possible, since the object of the present invention is a system containing mixed powders of two active materials (lithium oxide and lithium hydroxide) enclosed in a suitable envelope defining a volume V, only partially filled by such powders.
• FIG 2 shows a cross-sectional view of an alternate embodiment of a composite getter system 20 in which, differently from the system shown in Figure 1 , the lithium oxide particles 11, 11 ', 11 " and lithium hydroxide particles 12, 12', 12" are dispersed in a polymeric binder 23, indicated in grey.
• the employed powders have dimensions that are usually determined and controlled by means of a sieving operation, and owing also to the geometrical conformation of the powders (not regular/spherical), this ensures that are selected and employed all the powders that have a minimal size lesser than the sieve opening.
• the present invention for both active materials when they are employed as such, are usefully employed particles/powders whose minimal size is higher than 1 ⁇ .
• the preferred powders distribution is comprised between 1 and 250 ⁇ (minimal size of the powders), this allows for an easier manufacturability of systems with the desired thicknesses.
• a polymeric binder particularly advantageous is the use of High Density Polyethylene (HDPE) or Polypropylene (PP), Low Density Polyethylene (LDPE), copolymer ethylene-octene, polyolefm modified with maleic anhydride, Ethylene Vinyl (EVA), Styrene-Ethylene- Butadiene-Styrene (SEBS), Ethylene Propylene Diene Monomer (EPDM), Thermoplastic Elastomer (TPE) and combinations thereof.
• HDPE High Density Polyethylene
• PP Polypropylene
• LDPE Low Density Polyethylene
• EVA Ethylene Vinyl
• SEBS Styrene-Ethylene- Butadiene-Styrene
• EPDM Ethylene Propylene Diene Monomer
• TPE Thermoplastic Elastomer
• the thickness of the carbon dioxide permeable envelope is usefully comprised between 5 and 500 ⁇ . It is to be underlined that such thickness represents the mean value, since certain points of the envelope (sealing regions) may present a different thickness (typically higher).
• the thickness of the binder containing the powders shall be comprised between 50 and 400 ⁇ , and in any case shall not be less than at least 1,5 times the minimum dimension of the employed powders.
• binders may also be used to make the enclosing CC permeable envelope for both embodiments (free powders, polymer bound powders), in certain more demanding applications, such as in the case of rechargeable lithium batteries, the use of High Density Poly Ethylene (HDPE) and PolyPropylene (PP) being preferred.
• HDPE High Density Poly Ethylene
• PP PolyPropylene
• the LiOH/Li 2 0 molar ratio for the getter systems according to the present invention is to be evaluated, considered and determined for a "fresh" getter system, i.e. a getter system not yet exposed to high levels of C0 2 (and therefore consumed).
• the getter systems according to the present invention are the ones that exhibit the correct ratio between lithium hydroxide and lithium oxide when the molar content of lithium carbonate over the sum of the lithium oxide and lithium hydroxide is less then 25%.
• a preferred solution for the getter system according to the present invention envisions the use of a drying element, that advantageously is made by a dispersion of a moisture sorber in a suitable binder, e.g. a polymeric matrix. This further ensures that toward the end of the life there is no moisture release from the C0 2 getter system. It is to be underlined that the amount of the moisture sorber added in this case is much smaller than in other conventional systems when the lithium hydroxide is associated with another moisture-sorbing element.
• Suitable materials for the H 2 0 removal are for example alkaline-earth metal oxides, with particular reference to MgO, CaO and alumino silicates, such as zeolite.
• the invention consists in a sealed system containing an improved C0 2 composite getter comprising a C0 2 -permeable envelope having an internal volume V, containing powders of a first and a second active materials, characterized in that said first active material is lithium hydroxide and said second active material is lithium oxide, and the LiOH/Li 2 0 molar ratio is less than 1,5.
• said sealed systems are energy storage devices such as rechargeable Li-Ion batteries and supercapacitors.
• the C0 2 getter system contains between 5 and 500 milligrams of active material powders, such quantity may be higher and scale up depending also on the size of the sealed system, for example rechargeable Li-Ion batteries or supercapacitors may vary greatly in their internal volume and therefore need and can accommodate a higher quantity of getter material.
• a getter system according to the present invention was made by mixing 11,5 milligrams of LiOH and 34,5 milligrams of Li 2 0 powders (minimum size less than 100 ⁇ ) and putting them in a C0 2 -permeable envelope made of HDPE, with a thickness of 10 ⁇ .
• the internal Vm/V ratio was 0,25.
• a 47 wt% dispersion of LiOH+Li 2 0 in HDPE is produced in an extruder.
• a sample according to the present invention is made by enclosing an extruded sample of 53,5 mg and 1 x 1,5 cm x 230 ⁇ in size in a 10 ⁇ - ⁇ HDPE envelope and its weight increase after C0 2 exposure, as per Example 1, is monitored and recorded. The results of this tests are shown in Figure 4, dotted line 3.

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• 2012
  • 2012-07-11 IT IT001207A patent/ITMI20121207A1/it unknown
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