WO2010100599A1 - Batterie à film mince de grande capacité et son procédé de fabrication - Google Patents

Batterie à film mince de grande capacité et son procédé de fabrication Download PDF

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Publication number
WO2010100599A1
WO2010100599A1 PCT/IB2010/050881 IB2010050881W WO2010100599A1 WO 2010100599 A1 WO2010100599 A1 WO 2010100599A1 IB 2010050881 W IB2010050881 W IB 2010050881W WO 2010100599 A1 WO2010100599 A1 WO 2010100599A1
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WIPO (PCT)
Prior art keywords
wires
recited
battery
substrate
skeleton structure
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Ceased
Application number
PCT/IB2010/050881
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English (en)
Inventor
Erik Petrus Antonius Maria Bakkers
Rogier Adrianus Henrica Niessen
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.)
Koninklijke Philips NV
US Philips Corp
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Koninklijke Philips Electronics NV
US Philips Corp
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Publication of WO2010100599A1 publication Critical patent/WO2010100599A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0421—Methods of deposition of the material involving vapour deposition
    • H01M4/0428—Chemical vapour deposition
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • 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
    • H01M4/0421—Methods of deposition of the material involving vapour deposition
    • H01M4/0423—Physical vapour deposition
    • 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
    • H01M4/13—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
    • 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
    • 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
    • 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

  • This disclosure relates to thin- film batteries, and more particularly to methods and batteries so formed using surface enlargement to provide high capacity functionality.
  • Micro power sources such as all-solid-state thin film batteries (TFBs) are currently seen as the future power sources in many stand-alone and small-scale autonomous devices like sensor systems, RFID, medical implants and many more applications.
  • TFBs are of a planar nature (2D) and can thus only store a relatively small amount of energy per footprint area (-50 microAh/cm 2 per micron of cathode thickness).
  • Li can be intercalated into Si at a high concentration (4.4 Li atoms per Si atom), giving a theoretical energy capacity of about 4000 mAh/gr of Si.
  • the expansion of the Si layer upon Li intercalation results in a degradation of the layer, and limits the number of cycles.
  • diffusion through thick Si layers is slow and limits the operation performance (power output and charging speed) of the battery.
  • the surface enlargement (and thus energy/power output enhancement), which can be realized by means of providing the substrate with a plurality of cavities, is generally done by dry etching processes such as Reactive Ion Etching and Ion Beam Etching, which are expensive and slow. Further, the etch rate drops dramatically when very high aspect ratio structures (e.g., very deep cavities) need to be processed. Moreover, the tool costs and investment are also very high.
  • an all-solid-state thin film energy source with very high energy storage properties per footprint area is provided. This can be realized through 3D surface enlargement of a bottom substrate.
  • a highly-controllable nanowire structure is grown for creating a 3D backbone or skeleton structure on a planar substrate. This backbone can be covered by a complete thin film battery stack.
  • a battery comprising, e.g., LiMOx cathodes, solid-state electrolytes and Li-intercalation anodes (such as LiAl, LiSi, LiIn, LiZn, ...) may be employed.
  • planar battery systems result from surface area enlargement generated by selectively etching 3D features in standard planar substrates by means of reactive ion etching (RIE) for example.
  • RIE reactive ion etching
  • the present principles instead grow nanowires up from a substrate rather than etching structures into the substrate. Additionally, the surface coverage or wire density can be tuned accurately in a wide range (from 0.1% to over 50%).
  • One advantage is that by using a skeleton structure, the battery stack does not suffer from degradation upon cycling, as the active intercalation/storage electrodes can remain very thin. This implies that employing surface area enlargement results in a battery device in which the same amount of energy can be stored per footprint (as compared to planar geometries), using thinner active electrodes. This is combined with a very high storage capacity, stability and fast diffusion through the thin active layers.
  • Applications in which this power source can be utilized may include, for example, autonomous sensors for body area networks (BAN) and wireless sensor networks (WSN), lighting applications (presence detection), medical implants, etc.
  • a Vapor-Liquid-Solid (VLS) growth mechanism for semiconducting nanowires provides a mechanism for growing wires, e.g., from group IV, IH-V and II- VI compound semiconductor materials. Other materials such as conductive materials and even insulating materials may also be employed for wires.
  • the process controls impurity doping (p- and n-type), growth rate in the vertical and radial direction, and the fabrication of heterostructures.
  • p- and n-type impurity doping
  • the expansion of the crystal is accommodated by the geometry and diffusion is fast across short distances.
  • a storage capacity of, e.g., 3000 mAh/gr can be provided by such a system.
  • the wires may show degradation after several charge/discharge cycles due to a collapse of the wire structures. Therefore, protection structures and formation methods are provided in accordance with the present principles to provide a robust skeleton structure to support a high performance and reliable thin film battery.
  • a method for fabricating a battery includes growing wires on a substrate to form a three-dimensional skeleton structure to increase a surface area.
  • a battery stack is deposited on the skeleton structure and includes thinner active electrodes, which increases stability and a lifetime of the battery.
  • a method for fabricating a battery includes growing wires on a substrate to form a three-dimensional skeleton structure.
  • the skeleton structure resists degradation due to intercalation cycling and an active intercalation material is deposited on the skeleton structure.
  • a thin film battery (TFB) includes a substrate, and a plurality of vertical vapor- liquid-solid (VLS) grown nanowires attached to the substrate to form a three-dimensional skeleton structure. The skeleton structure resists degradation due to intercalation cycling.
  • a shell layer is formed over the wires and preferably forms an active electrode of a battery stack.
  • the battery stack is deposited on the skeleton structure.
  • the battery stack includes an active intercalation material.
  • the shell layer may be an anode or cathode of the battery.
  • the anode may be defined as a negative electrode of the battery (e.g., the active electrode of the battery having the most negative potential). This is because in a rechargeable battery system the word anode or cathode actually depends on the whether the battery is being charged or discharged.
  • FIG. 1 is a diagram showing a formation of a catalyst particle and the growth of a nanowire in accordance with the present principles
  • FIG. 2 is a cross-sectional view of a nanowire having a shell layer and optional barrier layer formed thereon;
  • FIG. 3 is a cross-sectional view of a skeleton structure of grown nanowires in accordance with the present principles
  • FIG. 4 is a cross-sectional view of the skeleton structure of FIG. 3 with a battery stack formed thereon in accordance with the present principles
  • FIG. 5 is a diagram showing a formation of catalyst particles on sides of nanowires and grown to form branches in accordance with the present principles.
  • FIG. 6 is a flow diagram showing steps for fabricating a battery in accordance with an illustrative embodiment.
  • the present disclosure describes an all-solid-state thin film energy source with very high energy storage properties per footprint area realized through 3D surface enlargement of the (bottom) substrate.
  • Highly-controllable nanowire growth is employed for creating a 3D backbone or skeleton structure on a planar substrate.
  • the surface coverage or wire density can be tuned accurately in a wide range (from 0.1% to over 50%). Due to the inert nature of the skeleton material, the structure does not suffer from degradation upon cycling. This is combined with a very high storage capacity, stability and fast diffusion, which are achieved through the thin active layers.
  • FIG. 1 a diagram depicts stages of nanowire growth on a substrate 10.
  • Substrate 10 may include any suitable material that is compatible with the nanowires material selection.
  • the substrate 10 may include an isolation material a conductive material or a semiconductive material, e.g., Si, Ge, GaAs, etc.
  • VLS Vapor- Liquid-Solid
  • the temperature for growth may be, e.g., about 400 - 450 0 C (preferably about 420 0 C).
  • the VLS mechanism condenses a vapor to form catalyst particles 12 on substrate 10.
  • the droplets or particles 12 settle to become elliptical in shape 14 to provide a position for growing nanowires 18.
  • a deposition of the material for forming nanowires 18 causes the nanowires to grow below particles 14. As time 16 elapses, the nanowires 18 grow larger.
  • These nanowires 18 have a small diameter (preferably about 20- 50 nm) and grow to between about a hundred nm to several microns.
  • a doping type and density of the nanowires 18 is controlled, such that in one embodiment we have at least about 10 19 cm "3 free carriers to have a conductive system. Controlling the doping density and doping type is performed by adjusting in-situ processing parameters, such as the type of doping element and temperature of evaporation, etc.
  • the material of a first layer which forms the nanowires 18 may be from group IV, IH-V or II- VI.
  • group III- V materials may include, e.g., GaN or InP.
  • a group II- VI compound may include, e.g., ZnO. Growth of the nanowire skeleton (e.g. wires 18) is terminated by decreasing the temperature and discontinuing a precursor flow.
  • a shell layer 22 is formed around the vertical nanowires 18.
  • the temperature may be greater than 420 0 C, but depends on the material selected for the shell layer 22.
  • the thickness of layer 22 is controlled by the deposition time, and the layer 22 may include any semiconductor material, for example, Si, Ge, another group IV element, a II- VI material or III-V material may be employed.
  • a deposition of a Sb shell e.g., about 10 nm in thickness
  • Si core nanowire 18
  • the shell layer 22 preferably forms an active electrode of a TFB battery stack.
  • the shell layer 22 is not an active battery electrode may include a situation where a non-doped skeleton structure is employed with a doped shell layer that can be utilized as a current collector, or the shell layer may be employed as a barrier layer.
  • Table 1 Lithium Insertion and Extraction Voltages are shown for selected materials.
  • a Si core/skeleton structure is covered with a Sb shell, then operating this (anode) structure in a voltage range (vs. a Li/Li + reference couple) from 0.8V - 1.2V, one can reversibly store Li in the Sb shell, but not in the Si core (as this reversibly stores lithium in the 0.25 - 0.45V range).
  • the core/shell structure material can be selected to provide a desired response for a battery in a desired voltage range.
  • the shell layer 22 is used as an active electrode material that reversibly stores lithium, while the core material 18 is electronically conductive as it is used as a current collector.
  • any semiconductor material may be employed for the core material 18, and preferably a doped semiconductor material.
  • carbon nanotube/wires (which reversibly store Li between 0 - 0.3V) may be grown on a substrate using VLS growth.
  • the carbon nanotubes/wires can be covered with a shell material that reversibly interacts with Li at potentials higher than that of carbon.
  • the shell layer 22 protects the wires 18 from degradation and collapse during charge/discharge cycles of intercalation cycling. Protection is provided by shell layer 22 to provide a robust skeleton structure to support a high performance and reliable thin film battery.
  • an effective lithium barrier layer 24, such as Ta, Ti, TaN or TiN can be deposited on the core wires 18 (preferably before depositing the shell layer 22) to prevent Li diffusion into the wire structure (and the accompanying volume changes).
  • This TiN/Ta barrier layer 24 is impenetrable to, e.g., Li, but is an electronic conductor and therefore is a good current collector as well as a barrier layer.
  • barrier layer 24 to chemically separate the core 18 and the shell 22 (or active electrode layers), a wide range of material combinations becomes possible, even those materials where the thermodynamics dictates that reversible Li storage of shell layer materials will occur at potentials more negative than those related to Li storage potentials of the core material.
  • Catalyst 14 may remain embedded in the structure.
  • the catalyst 14 can be removed, e.g., using a wet chemical etch based on, e.g., cyanide (CN " ) or iodide (I3 ).
  • the surface-enhanced substrate 30 is ready for the next step.
  • the surface- enhanced substrate 30 can subsequently be used to deposit a full battery stack 40 thereupon.
  • the battery stack 40 comprises formation of battery stack components, such as back-to-back layer depositions of an anode, a solid electrolyte and a cathode (or vise versa).
  • One of active electrodes (a cathode or an anode) of a battery stack may be formed as the shell layer 22.
  • a low pressure deposition technique may be employed.
  • This technique may include, e.g., a Low Pressure Chemical Vapor Deposition (LPCVD), an Atomic Layer Deposition (ALD) or special types of Physical Vapor Deposition (PVD), such as, biased sputtering.
  • the battery stack 40 may include, e.g., LiMOx cathodes, solid-state electrolytes and Li-intercalation anodes (such as LiAl, LiSi, LiIn, LiZn, ).
  • step conformal anodes silicon
  • solid electrolytes LIsPO 4
  • cathodes LiCo ⁇ 2
  • Other materials and processes may also be employed.
  • the present principles employ highly-controllable nanowire growth for creating a 3D backbone or skeleton structure on a planar substrate, which can additionally be covered by a layer of active (Lithium intercalation) material, e.g., solid electrolytes (LiSPO 4 ) and cathodes (LiCo ⁇ 2 ) of a battery stack.
  • active (Lithium intercalation) material e.g., solid electrolytes (LiSPO 4 ) and cathodes (LiCo ⁇ 2 ) of a battery stack.
  • the surface coverage or wire density can be tuned accurately in a wide range (from about 0.1% to over 50%).
  • the tuning of the wire density may be controlled by chamber temperature and pressure during catalyst deposition/formation (12, 14). Further, the wire density may be controlled by creating conditions for forming a 3D skeleton. This may include depositing a second generation of catalyst particles on side walls of the nanowires and growing branches.
  • Catalysts used for either or both of the first and second generations may include Au, Ag, Cu, Ni, Fe, Co (transition metals), etc., preferably metals with a low melting temperature.
  • catalyst materials may comprise the same element(s) as the nanowires 18 to be grown, such as, e.g., Ga, In, Zn, Al, etc.
  • branches 54 are grown outward from the nanowire 18. This provides a greater topography and may increase the surface area of the skeleton employed for forming a thin- film battery.
  • the structure which may be employed in batteries, does not suffer from degradation upon intercalation cycling, and provides a very high storage capacity, stability and fast diffusion through the thin active layers.
  • FIG. 6 a method for fabricating a battery in accordance with an illustrative embodiment is depicted.
  • a substrate is provided.
  • wires are grown on the substrate to form a three-dimensional skeleton structure.
  • the skeleton structure resists degradation due to intercalation cycling through material selection.
  • a vapor- liquid-solid (VLS) mechanism is employed to grow the wires from the substrate.
  • the VLS mechanism includes depositing catalyst particles on the substrate and growing the wires in a substantially vertical form at the sites of the catalyst particles.
  • the wires are preferably nanowires and have a diameter of between about 20nm and 50 nm.
  • the wires include at least one of a group IV material, a II-IV material, a III-V material, and/or suitable combinations thereof.
  • the wires may include at least one of GaN, InP and ZnO.
  • the wires on the substrate are formed at a first temperature, which is preferably less than or equal to 420 degrees Celsius.
  • a density of the wires is tunable in accordance with process parameters. The density can be adjusted from between about 0.1% to about 50%.
  • a second deposition of catalyst particles may be formed on sides of the wires and the VLS mechanism is again applied to form branches from the sides of the wires.
  • doping type and density of the wires is controlled to ensure conductivity in the wires.
  • a barrier layer is optionally formed over the wires that ensures that no electrochemically active species (which may include Li(O) or Li+ in the case of lithium-ion batteries) can diffuse from active intercalation material which would be subsequently formed onto the underlying skeleton structure (e.g., a shell layer).
  • a battery stack is formed over the wires of the skeleton structure.
  • the battery stack layer includes a shell layer.
  • the shell layer is formed in contact with the barrier layer or the wires of the skeleton structure.
  • the shell layer may include at least one of Si, Ge, and a III- V material if the wires are formed from II-IV material or a III -V material.
  • the shell layer includes an active intercalation material deposited on the barrier layer/skeleton structure.
  • the active intercalation material may include a lithium compound, and is preferably part of a battery stack formed over the skeleton structure.
  • the shell layer preferably forms a first active electrode, followed by an electrolyte and a second active electrode to form the battery stack.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

L'invention porte sur un procédé de fabrication d'une batterie qui comprend la croissance (104) de fils sur un substrat afin de former une structure de squelette tridimensionnelle pour augmenter une surface utile. Un empilement de batteries est déposé (116) sur la structure de squelette et peut être plus mince pour augmenter la stabilité et la durée de vie de la batterie.
PCT/IB2010/050881 2009-03-04 2010-03-01 Batterie à film mince de grande capacité et son procédé de fabrication Ceased WO2010100599A1 (fr)

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US15725709P 2009-03-04 2009-03-04
US61/157,257 2009-03-04

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