EP4104218A2 - Électrode, son utilisation, accumulateur et procédé de fabrication d'une électrode - Google Patents

Électrode, son utilisation, accumulateur et procédé de fabrication d'une électrode

Info

Publication number
EP4104218A2
EP4104218A2 EP21708916.8A EP21708916A EP4104218A2 EP 4104218 A2 EP4104218 A2 EP 4104218A2 EP 21708916 A EP21708916 A EP 21708916A EP 4104218 A2 EP4104218 A2 EP 4104218A2
Authority
EP
European Patent Office
Prior art keywords
layer
porous silicon
electrode
silicon substrate
silicon layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP21708916.8A
Other languages
German (de)
English (en)
Inventor
Benedikt STRAUB
John BURSCHIK
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
RENA Technologies GmbH
Original Assignee
RENA Technologies GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by RENA Technologies GmbH filed Critical RENA Technologies GmbH
Publication of EP4104218A2 publication Critical patent/EP4104218A2/fr
Pending legal-status Critical Current

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Classifications

    • 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
    • H01M4/139—Processes of manufacture
    • H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/12—Semiconductors
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/02—Etching
    • C25F3/12—Etching of semiconducting materials
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • H01M4/044—Activating, forming or electrochemical attack of the supporting material
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • H01M4/044—Activating, forming or electrochemical attack of the supporting material
    • H01M4/0445—Forming after manufacture of the electrode, e.g. first charge, cycling
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • H01M4/045—Electrochemical coating; Electrochemical impregnation
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • H01M4/045—Electrochemical coating; Electrochemical impregnation
    • H01M4/0452—Electrochemical coating; Electrochemical impregnation from solutions
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/049—Manufacturing of an active layer by chemical means
    • H01M4/0492—Chemical attack of the support material
    • 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
    • H01M4/134—Electrodes based on metals, Si or alloys
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/661—Metal or alloys, e.g. alloy coatings
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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 invention relates to an electrode, in particular for a lithium-ion accumulator, and its use.
  • the invention also relates to an accumulator and a method for producing an electrode.
  • Lithium-ion accumulators are a widespread type of accumulator and are used in a variety of devices, especially in mobile devices or in electric vehicles,
  • an electrode containing graphite is often used as the anode. Due to the comparatively low lithium absorption capacity of graphite, such an electrode has a limited specific charging capacity of up to 500 mAh / g,
  • silicon An alternative to graphite as an electrode material is silicon.
  • silicon-based electrode With a silicon-based electrode, a specific charging capacity of 4200 mAh / g can theoretically be achieved.
  • silicon has the disadvantage that when the lithium is stored, the silicon expands considerably. If a silicon-based electrode is used in a lithium-ion battery, the large volume expansion of the silicon can destroy the battery after a few charging cycles.
  • the invention is based on the object of providing an electrode which can achieve a high specific charging capacity and a long service life, as well as specifying a method for producing such an electrode.
  • this object is achieved according to the invention by an electrode according to claim 1.
  • this object is achieved according to the invention by a method according to claim 6.
  • the invention is also based on the object of providing an accumulator which can achieve a high specific charging capacity and a long service life.
  • the electrode according to the invention has at least one porous silicon layer and one copper layer.
  • the pores of the at least one silicon layer enable the silicon to expand into the cavities formed by the pores in the event of a volume expansion, for example when lithium is embedded. This enables the silicon to withstand the volume expansion undamaged, so that a long service life of the electrode can be achieved.
  • the at least one porous silicon layer can be produced with little effort.
  • their manufacture it is For example, it is possible to dispense with a masking step and / or multi-stage etching processes.
  • the at least one porous silicon layer can be manufactured at low cost, it is advantageously possible to manufacture the entire electrode with little effort.
  • the at least one porous silicon layer is preferably designed as a sponge-like structure.
  • the pores of the at least one porous silicon layer advantageously have a pore size of at least 10 nm. This makes it possible for the silicon to have sufficiently large cavities to allow for a volume expansion to survive undamaged. It is also advantageous if the pores have a pore size of at most 10,000 nm, in particular since larger pores can possibly have a disadvantageous effect on the stability of the at least one porous silicon layer.
  • the at least one porous silicon layer can be at least partially embedded in the copper layer. That is to say, the copper layer can be designed in such a way that it extends into at least some pores of the at least one porous
  • Silicon layer extends into it.
  • the copper layer is preferably arranged on the at least one porous silicon layer, in particular directly on the at least one porous silicon layer.
  • the copper layer has a layer thickness of at least 1 ⁇ m, preferably at least 2 ⁇ m.
  • a minimum layer thickness of the copper layer has an advantageous effect in the production process of the electrode, in particular since such a minimum layer thickness of the copper layer enables easier joint removal of the copper layer and the allows at least one porous silicon layer from a silicon substrate.
  • the layer thickness of the copper layer is at most 20 ⁇ m, preferably at most 12 ⁇ m, in particular since a layer thickness of the copper layer of more than 20 ⁇ m can possibly have a detrimental effect on the mechanical flexibility of the electrode.
  • the electrode comprises a multilayer system made up of several, preferably superposed, porous silicon layers to which the at least one porous silicon layer belongs. These can differ from one another, for example, in that the porous silicon layers each have different porosities and / or different pore sizes and / or pore shapes.
  • the copper layer of the electrode is preferably arranged on one of the porous silicon layers of the multilayer system, in particular directly on one of the porous silicon layers of the multilayer system.
  • the electrode is advantageously designed as a film, in particular as a rollable film.
  • An embodiment of the electrode as a roll-up foil makes it possible, for example, to use the electrode in the rolled-up state in an accumulator with a cylindrical design.
  • the film can be foldable. In this way, a rechargeable battery can be implemented with a design which, for example, has a rectangular base area.
  • the Electrode lithium is embedded. If the electrode is on
  • the method according to the invention for producing the electrode according to the invention comprises the following method steps:
  • the silicon substrate can, for example, be etched using a wet chemical method. That is to say that the etching of the silicon substrate can in particular be a wet chemical etching.
  • the silicon substrate can be etched for the purpose of forming the at least one porous silicon layer in a so-called batch process, for example by etching the silicon substrate in an immersion bath.
  • the etching takes place for the purpose of forming the at least one porous silicon layer in a continuous process, whereby, for example, the production of a large number of inventive
  • Electrodes is made possible with little time and effort.
  • the silicon substrate is preferably etched on one side for the purpose of forming the at least one porous silicon layer.
  • the silicon substrate is electrochemically etched for the purpose of forming the at least one porous silicon layer,
  • the silicon substrate can, for example, be transported along a transport direction over a plurality of treatment basins arranged one behind the other in the transport direction, each of which is filled with an etching medium and in each of which an electrode is arranged.
  • the silicon substrate preferably comes into contact with the etching medium located in the respective treatment basin on its substrate underside during transport over the treatment basin. It is also advantageous if the polarity of the electrodes arranged in the treatment basin alternates in the direction of transport.
  • the polarity of the electrodes arranged in the treatment basin alternates in the transport direction can be understood to mean that a positively charged electrode is followed by a negatively charged electrode in the transport direction and another positively charged electrode follows the negatively charged electrode in the transport direction Such a polarity change is correspondingly repeated in the case of more than three treatment basins following one another in the transport direction. The same applies in the event that the first electrode is a negatively charged electrode.
  • a gas nozzle can be arranged between two treatment basins, by means of which a gas or a gas mixture, such as air, is blown onto the underside of the substrate in order to remove the etching medium located on the underside of the substrate.
  • the gas nozzle can in particular be designed as a so-called air knife (also known as an “air knife”)
  • Protective gas in particular nitrogen, is blown onto the underside of the substrate. In this way, increased oxidation of the substrate and the associated increased risk of breakage can be avoided.
  • the silicon substrate is preferably subjected to an electrical current density of at least 0.5 mA / cm 2 , in particular at least 1 mA / cm 2 . It is also preferred if the electrical current density with which the silicon substrate is subjected during electrochemical etching is at most 200 mA / cm 2 , in particular at most 120 mA / cm 2 .
  • the etching medium with which the treatment basins are filled preferably contains hydrogen fluoride.
  • the etching medium can be an aqueous hydrogen fluoride solution.
  • the etching medium can optionally contain a surfactant and / or an additive.
  • the etching can be carried out for the purpose of forming the at least one porous silicon layer, in particular as a metal-catalyzed chemical etching process (also called “metal assisted etching” in specialist circles).
  • the deposition of the copper layer on the at least one porous silicon layer can take place in different ways.
  • the copper layer can be deposited on the at least one porous silicon layer by means of sputtering a copper target using ions (also known as “ion sputtering”).
  • the copper layer can be deposited on the at least one porous silicon layer, for example by applying a copper paste by means of screen printing and / or a rolling process. It is also possible lent to deposit the copper layer on the at least one porous silicon layer by a chemical deposition process.
  • the copper layer can be deposited in a two-stage process. For example, in a first deposition step, a first part of the copper layer can be deposited on the at least one porous silicon layer by means of galvanic displacement (also called "galvanic displacement" in specialist circles). In a second deposition step, a second part can then be deposited The copper bar can be deposited on the first part of the copper bar by means of electrochemical deposition.
  • Such a two-stage process can form a homogeneous and robust copper bar.
  • the first deposition step in particular, it can be avoided that it occurs as a result of the high electrical resistance
  • the electrochemical deposition of the at least one porous silicon layer or the multilayer system leads to island formation of copper, which would result in an inhomogeneous copper layer.
  • the respective deposition step can be implemented as a batch process or as a continuous process.
  • a Niekel layer is deposited on the at least one porous silicon layer in a first deposition step.
  • the copper layer is then deposited on the Niekel layer in a second deposition step.
  • the adhesion of the copper layer following the Niekel layer to the silicon layer can be improved.
  • the deposition of the nickel layer in the first deposition step on the at least one porous silicon layer can be carried out in accordance with one of the previous steps in connection with the deposition of the copper layer on the at least one porous silicon layer procedures described.
  • the nickel layer is preferably deposited on the at least one porous silicon layer by means of electrochemical deposition.
  • the silicon substrate is preferably subjected to an electrical current density of at least 0.5 mA / cm 2 , in particular an electrical current density of at least 10 mA / cm 2 .
  • the silicon substrate is advantageously subjected to an electrical current density of at most 150 mA / cm 2 , preferably of at most 100 mA / cm 2 , for the purpose of forming the nickel layer.
  • the nickel layer has a layer thickness of at least 0.1 ⁇ m, preferably of at least 0.5 ⁇ m. It is also advantageous if the layer thickness of the nickel layer is at most 3 ⁇ m, preferably at most 1.5 ⁇ m.
  • the copper layer can be deposited on the nickel layer by means of electrochemical deposition.
  • the respective separation step can be implemented as a batch process or as a continuous process.
  • Galvanic displacement is a self-limiting process.
  • the first part of the copper layer or the nickel layer can in particular be used as an electrically conductive seed layer, i. H. serve as a conductive substrate for the formation of the second part of the copper layer, which is deposited in the second deposition step by means of electrochemical deposition.
  • the silicon substrate is preferably coated with a Separation solution, in particular an aqueous separation solution, brought into contact.
  • a Separation solution in particular an aqueous separation solution
  • the deposition solution can contain, for example, copper sulfate, in the case of the deposition of the Niekel layer, for example, nickel sulfate or nickel sulfamate.
  • the separation solution can also contain hydrogen fluoride.
  • the deposition solution can contain an additive, in particular an organic additive, for better surface wetting of the silicon substrate, for setting the pH value and / or for homogenizing the ash separation solution.
  • the silicon substrate is advantageously wetted with a deposition solution.
  • a deposition solution This preferably contains copper sulfate.
  • an electrical current is applied between the silicon substrate and the last-mentioned deposition solution Part of the copper layer is subjected to an electrical current density of at least 0.5 mA / cm 2 , in particular at least 1 mA / cm 2.
  • the first part of the copper layer deposited on the silicon substrate is used for the purpose of switching off - Images of the second part of the copper layer with an electrical current density of at most 150 mA / cm 2 , in particular at most 100 mA / cm 2 , is applied.
  • the nickel layer in which the copper layer is deposited on the nickel layer, the nickel layer can be subjected to the current densities mentioned for the purpose of depositing the copper layer.
  • the electrical current density with which the first part of the copper layer or the nickel layer is applied for the purpose of depositing the second part of the copper bar or the copper layer can be set so that the electrical current density is constant over time.
  • the electrical current density can be set in such a way that the electrical current density increases according to a predetermined ramp or alternates over time. The latter enables the deposition of the second part of the copper layer, or the copper layer on the nickel layer, with an increasing or alternating deposition rate, for example in order to achieve better homogeneity of the copper layer.
  • a preferred development of the invention provides that by means of the etching of the silicon substrate, a multi-layer system is formed from several porous silicon layers, the at least one porous silicon layer being one of the several porous silicon layers of the multi-layer system.
  • the porous silicon layers can differ from one another, for example, in that the porous silicon layers each have different porosities and / or different pore sizes and / or pore shapes.
  • the individual porous silicon layers of the multilayer system can have different functions.
  • One of the silicon layers of the multilayer system can be provided as a release layer, for example.
  • One or more other silicon layers of the multilayer system can be used, for example, to store lithium.
  • Another one of the silicon layers of the multi-layer system can be provided as a barrier layer for the copper layer to be deposited.
  • the multilayer system is designed in such a way that that porous silicon layer of the multilayer system, which has the greatest porosity, directly adjoins a non-porosified part of the silicon substrate.
  • the porous silicon layer of the multilayer system, which has the greatest porosity is preferably used as a release layer, that is to say as a layer which serves to detach at least part of the multilayer system from the non-porosified part of the silicon substrate.
  • the at least one porous silicon slide is advantageously removed together with the copper bar from a non-porous part of the silicon substrate.
  • a multi-layer system is formed from several porous silicon layers, it is advantageous if several layers, in particular all layers, of the multi-layer system are removed together with the copper layer from the non-porous part of the silicon substrate.
  • the silicon substrate is preferably subjected to a thermal treatment.
  • the thermal treatment can take place, for example, by means of a furnace, in particular by means of a continuous furnace.
  • the thermal treatment can, for example, ensure that at least some of the pore walls of the at least one porous silicon layer and / or possibly at least some of the pore walls of one of the other porous silicon layers of the multilayer system, in particular the pore walls of that porous silicon layer which has the largest Has porosity, break in, so that the at least one porous silicon layer can be removed together with the copper layer from the non-porosified part of the silicon substrate in a cost-effective manner.
  • a temperature gradient is advantageously generated between the silicon substrate and its surroundings.
  • the temperature gradient can be generated in different ways, for example by heating plates and / or by infrared lamps and / or by circulating air heating and / or by induction heating,
  • the temperature gradient is preferably at least 20.degree. C., in particular at least 30.degree. C. It is also expedient if the temperature of the silicon substrate during the thermal treatment is kept below the melting temperature of silicon, in particular to avoid destruction of the porous Avoid structure of the at least one porous silicon layer.
  • a different method in particular a mechanical pull-off method, can be used instead of a thermal treatment.
  • lithium is incorporated into the at least one porous silicon layer.
  • a multi-layer system is formed from several porous silicon layers, it can in particular be provided that lithium is embedded in several or all of the porous silicon layers of the multi-layer system.
  • the lithium can be stored in elemental form, for example in the form of lithium clusters, and / or as part of a chemical compound, for example in the form of a lithium-silicon mixed crystal.
  • the lithium is preferably stored after the at least one porous silicon layer and possibly any other porous silicon layers together with the copper layer has / have been removed from the non-porous silicon substrate.
  • any metal residues such as copper residues or nickel residues and / or any residues can be more porous
  • Structures such as protruding stilts can be removed from the remaining silicon substrate. This makes it possible to recycle the remaining silicon substrate. For example, after any metal residues such as copper or nickel residues and / or any residues of porous structures have been removed, the remaining silicon substrate can be used to produce a further electrode, in particular by repeating the steps described above. Any residues of porous structures and / or any metal residues, such as copper residues or nickel residues, can be removed, for example, by means of a wet-chemical etching process, which can be implemented in particular as a batch process or as a continuous process.
  • both residues of porous structures and metal residues, such as copper residues or nickel residues, are to be removed, these are preferably removed by a two-stage etching process in which the remaining silicon substrate is placed in a first treatment tank filled with etching medium and then in a second, with another Treatment basin filled with etching medium is treated.
  • the metal residues such as copper residues or nickel residues
  • An acidic etching medium is preferably used to remove metal residues, such as copper residues or nickel residues. This can contain, for example, hydrogen fluoride and / or hydrogen chloride and / or nitric acid and / or sulfuric acid and / or an oxidizing agent such as hydrogen peroxide and / or ozone.
  • An alkaline etching medium or an acidic etching medium can be used to remove residues of porous structures.
  • the former can contain sodium hydroxide and / or potassium hydroxide, for example.
  • the latter can contain, for example, hydrogen fluoride and / or nitric acid and / or sulfuric acid.
  • any residues of porous structures and / or any metal residues can be removed in another way, for example by mechanical grinding and / or polishing and / or plasma etching and / or laser ablation.
  • the invention relates, inter alia, to a use of the electrode and an accumulator.
  • the electrode according to the invention is used according to the invention, it is provided that the electrode is used as an anode, preferably in an accumulator.
  • the electrode can be used particularly advantageously as an anode in a lithium-ion accumulator.
  • the electrode is preferably activated, for example by carrying out several charge-discharge cycles of the accumulator.
  • the charge-discharge cycles can in particular be carried out in accordance with one or more predetermined current-voltage curves.
  • By activating the electrode it can be achieved that, in particular as a result of self-organized recrystallization of the silicon, an island structure is formed in the at least one porous silicon layer, which does not develop further after a few cycles and is largely stable over further cycles remain. If the at least one silicon layer of the electrode were not porous, the electrode would be destroyed when the charge-discharge cycles are carried out.
  • Electrode in an accumulator a process step for structuring the electrode can be carried out.
  • the structuring of the electrode can take place, for example, as mechanical structuring by means of a negative mold, in particular a mask, roller and / or roller, and / or as laser structuring.
  • the accumulator according to the invention is equipped with the electrode according to the invention.
  • the accumulator is preferably a lithium-ion accumulator.
  • said electrode is designed as a rollable film.
  • a rollable film can be formed from a multiplicity of sections welded or glued to one another.
  • the electrode can be rolled or wound around an axis with further components of the accumulator, such as for example a further electrode and / or a separator.
  • the other components of the accumulator are also available as roll-up foils educated. In this way, a cylindrical shape of the accumulator can be realized.
  • the accumulator can be equipped with a folded electrode.
  • the other components of the accumulator can be folded between the electrode to form a stack.
  • the other components of the accumulator can be designed as individual sections and / or as foldable foils. If the other components of the accumulator are designed as foldable foils, they can be folded alternately with the electrode in the form of a foil by means of a Z-folding technique to form a stack. In the case of a Z-folding technique, folding as often as desired, but at least twice, can take place, each in a direction opposite to the previous folding direction. In this way, diverse design options for a design of the accumulator are made possible, for example a cuboid design.
  • the accumulator has a stack arrangement, in particular a cuboid stack arrangement, with cutouts, in particular rectangular sections, of the electrode and the other components of the accumulator stacked separately from one another.
  • FIG. 1 shows a treatment device for treating a substrate
  • FIG. 2 shows a sectional illustration of a silicon substrate treated with the treatment device from FIG. 1, which has a multilayer system made up of several porous silicon layers
  • FIG. 3 shows the silicon substrate from FIG. 2 in a view from below;
  • FIG. 4 shows the silicon substrate and a first part of a copper layer, which is cut off in a first deposition step on the silicon substrate, in one
  • FIG. 5 shows a sectional illustration of the silicon substrate and the copper layer deposited on the silicon substrate in two deposition steps
  • FIG. 6 shows the silicon substrate and the copper layer deposited on the silicon substrate after a joint Separating the copper layer and a plurality of porous silicon layers from a non-porosified part of the silicon substrate in a sectional view;
  • FIG. 7 shows a sectional illustration of an electrode for an accumulator which is formed by the separated copper layer, the separated porous silicon layers and lithium embedded in the porous silicon layers;
  • FIG. 8 shows a sectional illustration of one of the porous silicon layers of the electrode from FIG. 7 after activation of the electrode;
  • FIG. 9 shows the non-porosified part of the silicon substrate as well as metal residues and residues of porous structures located on the non-porosified part of the silicon substrate in a side view;
  • FIG. 10 shows the non-porosified part of the silicon substrate during the removal of the metal residues in an irrigation basin;
  • FIG. 11 shows the non-porosified part of the silicon substrate after the removal of the metal residues, the non-porosified part of the silicon substrate being located in a further treatment basin for removing the residues of porous structures;
  • FIG. 12 shows a lithium-ion accumulator, which is equipped with the electrode from FIG. 7, in a partial sectional illustration;
  • FIG. 13 shows an alternative design of a rechargeable battery with the electrode from FIG. 7;
  • FIG. 14 shows an alternative arrangement of the electrode from FIG. 7.
  • FIG. 1 shows a treatment device 1 for treating a substrate, in particular for one-sided electrochemical etching of a substrate.
  • FIG. 1 shows a silicon substrate 2 to be treated by means of the treatment device 1.
  • the treatment device 1 comprises a transport device 3 which is set up to transport the silicon substrate 2 to be treated along a transport direction 4.
  • the transport device 3 is designed as a roller conveyor with a plurality of transport tubes 5.
  • the treatment device 1 comprises a plurality of treatment basins 6 arranged one behind the other in the transport direction 4, each of which is filled with an etching medium 7 and in each of which an electrode 8 is arranged.
  • three treatment basins 6 are shown as an example. In principle, the treatment device 1 can have a larger or a smaller number of treatment basins 6.
  • the etching medium 7 is preferably an aqueous hydrogen fluoride solution.
  • the etching medium 7 can optionally contain an additive and / or a surfactant.
  • An electrical potential is applied to each of the electrodes 8, the polarity of the electrodes 8 alternating in the transport direction 4.
  • the silicon substrate 2 is moved over the treatment basin 6 along the transport direction 4 transported, the silicon substrate 2 only coming into contact with the etching medium 7 located in the treatment basin 6 on its substrate underside 9.
  • an electrochemical reaction takes place in which, as a result of local inhomogeneities in the electrical current density, etching peaks and valleys are formed, which leads to the formation of pores on the substrate underside 9, so that on the substrate underside 9 a porous structure is created.
  • the electrochemical reaction can be controlled via the electrical potential of the electrodes 8, which influences the electrical current density in the treatment basin 6.
  • the reaction can be controlled by adding an additive and / or a surfactant.
  • a hydrogen fluoride-containing such as an etching medium
  • the following reaction in particular occurs on the substrate underside 9: Si + 6F- + 4h + -> SiF 6 2- .
  • the electrical current provides defect electrons (ht) on the surface of the silicon substrate 2 and the hydrogen fluoride forms hydrogen fluoride ions (F-) in the solution.
  • the electrical current density in the treatment basin 6 can be set in such a way that the porous structure of the silicon substrate 2 is subdivided over the depth of the silicon substrate 2, so that several porous silicon layers are formed on the substrate underside 9, which differ in terms of their porosity and / or their pore size and / or their pore shapes differ from one another.
  • the treatment device 1 comprises an air knife, not shown in the figures, between the treatment basins 6, by means of which a gas flow 10 of nitrogen is generated to blow away the etching medium 7 located on the substrate underside 9.
  • FIG. 2 shows the silicon substrate 2 treated with the aid of the treatment device 1 from FIG. 1 in a sectional illustration.
  • the treated silicon substrate 2 has, on its substrate underside 9, a multilayer system 11 composed of a plurality of porous silicon layers 12a, 12b, 12c, 12d arranged one above the other.
  • a multilayer system 11 composed of a plurality of porous silicon layers 12a, 12b, 12c, 12d arranged one above the other.
  • four porous silicon layers 12a, 12b, 12c, 12d are shown by way of example, it being possible in principle to form a larger or smaller number of porous silicon layers on the substrate underside 9 of the silicon substrate 2 during the treatment with the aid of the treatment device 1.
  • the porous silicon layers 12a, 12b, 12c, 12d differ from one another with regard to the size of their pores 13 and / or the shape of their pores 13 and / or their porosity, with that porous silicon layer 12d of the multilayer system 11 which has the greatest porosity being directly affected a non-porosified part 14 of the silicon substrate 2 is adjacent.
  • This porous silicon layer 12d serves as a release layer for later removal of the multilayer system 11 from the non-porous part 14 of the silicon substrate 2 (cf. FIG. 6).
  • FIG. 3 shows the silicon substrate 2 from FIG. 2 in a view from below.
  • Figure 3 are several pores 13 of different shapes and
  • Multi-layer system 11 deposited a copper layer 15 in a two-stage deposition process (see FIGS. 4 and 5).
  • a first part 16 of the copper layer 15 is deposited on the multilayer system 11 by means of galvanic displacement.
  • the silicon substrate 2 is brought into contact on its substrate underside 9 with an aqueous deposition solution which contains hydrogen fluoride and copper sulfate.
  • the hydrogen fluoride dissolves silicon dioxide from the substrate underside 9 of the silicon substrate 2, so that unoxidized silicon remains on the substrate underside 9, which is very attractive for the copper ions contained in the deposition solution because of the chemical potential between silicon and copper.
  • the galvanic displacement is a self-limiting process that stops automatically when the outermost porous silicon layer 12a is completely covered with copper.
  • the said first part 16 of the copper layer 15 has been formed in such a way that the outermost porous silicon layer 12a is embedded in the first part 16 of the copper layer 15.
  • a second part 17 of the copper layer 15 is then deposited on the first part 16 of the copper layer 15 by means of electrochemical deposition.
  • the first part 16 of the copper layer 15 serves as an electrically conductive seed layer for the formation of the second part 17 of the copper layer 15.
  • the silicon substrate 2 is wetted on its substrate underside 9 with a deposition solution containing copper sulfate and an electric current is applied.
  • the silicon substrate 2 serves as a negatively charged electrode, while the deposition solution serves as a positively charged counter-electrode.
  • FIG. 4 shows a sectional illustration of the silicon substrate 2 after the deposition of the first part 16 of the copper layer 15 on the multilayer system 11.
  • FIG. 5 shows a sectional illustration of the silicon substrate 2 after the deposition of the second part 17 of the copper layer 15 on the first part 16 of the copper layer 15.
  • the silicon substrate 2 is subjected to a thermal treatment (cf. FIG. 6). This can take place, for example, in a continuous furnace, not shown in the figures.
  • heat radiation 18 causes the pore walls of the porous silicon layer 12d serving as a release layer (cf. FIGS. 2, 4 and 5) to collapse, which is due to the different thermal expansion coefficients between the porous silicon layers 12a, 12b , 12c on the one hand and the porous silicon layer 12d on the other hand can be returned.
  • the copper layer 15, together with the porous silicon layers 12a, 12b, 12c of the multilayer system 11, can be detached from the non-porosified part 14 of the silicon substrate 2.
  • porous silicon layer 12d serving as a detaching layer, only thin layers remain after the thermal treatment Stilts 19 left. These boundaries in each case on the non-porosified part 14 of the silicon substrate 2 or on the porous silicon layer 12c of the multilayer system 11 that was previously arranged adjacent to the release layer.
  • FIG. 6 shows the silicon substrate 2 and the copper layer 15 deposited on the silicon substrate 2 after a joint separation of the copper layer 15 and the porous silicon layers 12a, 12b, 12c from the non-porosified part 14 of the silicon substrate 2 in a sectional illustration.
  • lithium 20 is stored in the separated porous silicon layers 12a, 12b, 12c (see FIG. 7).
  • FIG. 7 shows a sectional illustration of an exemplary embodiment of an electrode 21 according to the invention for a storage battery, which is designed as a rollable film.
  • This electrode 21 is through the porous silicon layers 12a, 12b, 12c, the copper layer 15 and in the porous
  • Lithium 20 embedded in silicon layers 12a, 12b, 12c is formed.
  • the electrode 21 After the electrode 21 has been installed in an accumulator, the electrode 21 is activated by carrying out several charge-discharge cycles of the accumulator.
  • FIG. 8 shows a sectional illustration of one of the porous silicon layers 12a, 12b, 12c of the electrode 21 from FIG. 7 after the electrode 21 has been activated.
  • FIG. 8 the island structure of the depicted porous silicon layer formed from a plurality of rectangular areas 22 can be seen.
  • a copper layer is deposited by means of an alternative method variant on a multilayer system which corresponds to the multilayer system 11 described in connection with FIG.
  • a nickel layer is deposited on the multilayer system in a first deposition step.
  • the nickel layer is deposited on the multilayer system by means of electrochemical deposition.
  • the silicon substrate is wetted on its underside of the substrate with a deposition solution containing nickel sulfate or nickel sulfamate, and an electric current is applied.
  • Figure 4 can be used to illustrate the deposition of the nickel layer.
  • the reference symbol 16 would refer to the nickel layer.
  • the elements of the alternative exemplary embodiment correspond to the elements shown in FIG.
  • a copper layer is deposited on the nickel layer by means of electrochemical deposition.
  • the nickel layer serves as an electrically conductive seed layer for the formation of the copper layer and provides improved adhesion of the copper bar applied to the nickel layer on the porous silicon layer.
  • FIG. 5 illustrates the deposition of the copper layer on the Niekel layer.
  • the reference symbol 16 would refer to the Niekel layer and the reference symbol 17 would refer to the copper layer deposited on the Niekel layer.
  • FIGS. 1 to 8. Unless otherwise stated, they can also be combined without restriction with the alternative exemplary embodiment described above.
  • FIG. 9 shows the non-porosified part 14 of the silicon substrate 2 in a side view. Furthermore, in FIG. 9 there are residues of porous structures which are adjacent to the non-porosified part 14 of the silicon substrate 2 and are formed by thin stilts 19, as well as metal residues 23 located on the non-porosified part 14 of the silicon substrate 2, with those of the non-porosified part 14 of the silicon substrate 2 is contaminated during the deposition of the copper layer 15 according to the first embodiment described in connection with FIGS. 1 to 8 or during the deposition of the nickel layer and the copper layer according to the alternative embodiment.
  • the stilts 19 and the metal residues 23 are removed in a two-stage wet chemical etching process (cf. FIGS. 9 and 10).
  • the not poro- fied portion 14 of Si l iziumsubstrats 2, for example l ung a further electrode of the type described above are used for the manufacture, especially in the previously described method steps' are repeated.
  • FIG. 10 shows the non-porosified part 14 of the silicon substrate 2, the adjacent stilts 19, said metal residues 23 and a treatment basin 24.
  • the treatment basin 24 is filled with an acidic etching medium 25, which is used to remove the metal residues 23 in the form of copper in the case of the first embodiment or in the form of copper and nickel in the case of the alternative embodiment.
  • the etching medium 25 can contain hydrogen fluoride and / or hydrogen chloride and / or nitric acid and / or sulfuric acid and / or hydrogen peroxide and / or ozone.
  • FIG. 10 shows a state in which the non-porous part 14 of the silicon substrate 2 is immersed in the etching medium 25 and the said metal residues 23 are dissolved in the etching medium 25.
  • FIG. 11 shows the non-porosified part 14 of the silicon substrate 2 as well as a further treatment basin 26.
  • the treatment basin 26 from FIG. 11 is filled with an etching medium 27 which is used to remove the aforementioned stilts
  • This etching medium 27 can be an alkaline etching medium or an acidic etching medium.
  • the etching medium 27 can contain, for example, deionized water and sodium hydroxide and / or potassium hydroxide.
  • the etching medium 27 can, for example, hydrogen fluoride and / or nitric acid and / or sulfuric acid and / or hydrogen peroxide and / or 0zone.
  • FIG. 11 shows a state in which the non-porous part 14 of the silicon substrate 2 is immersed in the etching medium 27 located in the treatment basin 26.
  • the etching medium 27 effects a surface polishing of the silicon substrate 2, so that in this state the previously mentioned stilts 19 are removed from the non-porosified part 14 of the silicon substrate 2 and the non-porosified part 14 of the silicon substrate. 2 for a further production of an electrode of the previously described type can be used.
  • FIG. 12 shows an exemplary embodiment of an accumulator 28a according to the invention in a partial sectional illustration.
  • the accumulator 28a is a lithium-ion accumulator with a cylindrical design.
  • the accumulator 28a comprises a cylindrical housing 29a.
  • the accumulator 28a comprises a cathode 30a, an anode 31a and a separator 32a arranged between the cathode 30a and the anode 31a.
  • the cathode 30a, the anode 31a and the separator 32a are each formed as a rolled-up film and are arranged in the housing 29a of the accumulator 28a.
  • the anode 31a of the accumulator 28a is the previously described electrode 21 (see FIGS. 7 and 8). That is, the above-described electrode 21 is used as the anode 31a in the secondary battery 28a.
  • FIG. 13 shows an alternative embodiment of the accumulator described in connection with FIG. 12 in one
  • the accumulator 28b has an alternative design with a rectangular base area.
  • the accumulator 28b comprises a cuboid housing 29b.
  • the accumulator 28b comprises a cathode 30b, an anode 31b and a separator 32b arranged between the cathode 30b and the anode 31b.
  • the cathode 30b, the anode 31b and the separator 32b are designed as rectangular sections and are stacked in a predetermined order in the housing 29b of the accumulator 28b.
  • the anode 31b of the accumulator 28b is the previously described electrode 21 (see FIGS. 7 and 8). That is, the above-described electrode 21 is used in the secondary battery 28b as the anode 31b in the form of rectangular sections.
  • FIG. 14 shows an alternative possible arrangement of the cathode 30b, the anode 31b and the separator 32b in the form of a cuboid stack for the alternative exemplary embodiment of the accumulator 28b described in connection with FIG.
  • the anode 31b is designed as a foldable film.
  • the cathode 30b and the separator 32b are folded between the anode 31b by means of a Z-folding technique.
  • the cathode 30b and the separator 32b can be designed in pairs as rectangular sections.
  • the cathode 30b and the separator 32b are preferably designed as a foldable film.
  • a superimposed Z-folding technique can be used.
  • the anode 31b, the cathode 30b and the separator 32b can be folded into a cuboid stack in alternating folding steps. For example, in a first folding step, the cathode 30b and the separator 32b can be folded between the anode 31b.
  • the anode 31b can be folded between the separator 32b arranged in pairs with the cathode 30b.
  • the first folding step can be carried out again.
  • a cuboid design of the accumulator 28b can be produced inexpensively and / or in an automated manner.

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Abstract

L'invention concerne une électrode (21) notamment destinée à un accumulateur lithium-ion (28a; 28b). Selon l'invention, l'électrode (21) comporte au moins une couche de silicium poreuse (12a, 12b, 12c, 12d) et une couche de cuivre (15). L'invention concerne en outre un accumulateur (28a; 28b) pourvu d'une telle électrode (21), un procédé de fabrication d'une telle électrode (21) et l'utilisation d'une telle électrode (21) dans un accumulateur (28a; 28b).
EP21708916.8A 2020-02-11 2021-02-11 Électrode, son utilisation, accumulateur et procédé de fabrication d'une électrode Pending EP4104218A2 (fr)

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DE102020103531.4A DE102020103531A1 (de) 2020-02-11 2020-02-11 Elektrode, deren Verwendung, Akkumulator sowie Verfahren zur Herstellung einer Elektrode
PCT/DE2021/100137 WO2021160222A2 (fr) 2020-02-11 2021-02-11 Électrode, son utilisation, accumulateur et procédé de fabrication d'une électrode

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KR102861629B1 (ko) * 2024-06-03 2025-09-17 한화모멘텀 주식회사 음극재 및 이의 제조방법, 이를 포함하는 리튬이온 이차전지

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DE102020103531A1 (de) 2021-08-12
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