US20070082268A1 - Chemical protection of metal surface - Google Patents

Chemical protection of metal surface Download PDF

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Publication number
US20070082268A1
US20070082268A1 US11/457,525 US45752506A US2007082268A1 US 20070082268 A1 US20070082268 A1 US 20070082268A1 US 45752506 A US45752506 A US 45752506A US 2007082268 A1 US2007082268 A1 US 2007082268A1
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US
United States
Prior art keywords
carbons
groups
anode
halogens
alkyl
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.)
Abandoned
Application number
US11/457,525
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English (en)
Inventor
Kurt Star
John Muldoon
Filippo Marchioni
Fred Wudl
Bruce Dunn
Monique Richard
Kimber Stamm
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.)
Toyota Motor Engineering and Manufacturing North America Inc
University of California San Diego UCSD
Original Assignee
Individual
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
Priority to US11/457,525 priority Critical patent/US20070082268A1/en
Application filed by Individual filed Critical Individual
Assigned to THE REGENTS OF THE UNIVERSITY OF CALIFORNIA reassignment THE REGENTS OF THE UNIVERSITY OF CALIFORNIA ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: DUNN, BRUCE S., MARCHIONI, FILIPPO, STAR, KURT, WUHL, FRED
Assigned to Toyota Engineering & Manufacturing North America, Inc. reassignment Toyota Engineering & Manufacturing North America, Inc. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MULDOON, JOHN, RICHARD, MONIQUE, STAMM, KIMBER L.
Publication of US20070082268A1 publication Critical patent/US20070082268A1/en
Priority to CN2007800325285A priority patent/CN101542782B/zh
Priority to PCT/US2007/012613 priority patent/WO2008008130A2/en
Priority to KR1020097002913A priority patent/KR101501565B1/ko
Priority to JP2009519433A priority patent/JP5336363B2/ja
Assigned to TOYOTA MOTOR ENGINEERING & MANUFACTURING NORTH AMERICA, INC. reassignment TOYOTA MOTOR ENGINEERING & MANUFACTURING NORTH AMERICA, INC. CORRECTIVE ASSIGNMENT TO CORRECT THE ASSIGNEE PREVIOUSLY RECORDED ON REEL 018697 FRAME 0085. ASSIGNOR(S) HEREBY CONFIRMS THE CORRECT NAME OF THE ASSIGNEE IS TOYOTA MOTOR ENGINEERING & MANUFACTURING NORTH AMERICA, INC.. Assignors: MULDOON, JOHN, RICHARD, MONIQUE, STAMM, KIMBER L.
Priority to US12/396,223 priority patent/US20090220857A1/en
Priority to US14/156,241 priority patent/US20140134488A1/en
Priority to US14/163,536 priority patent/US8840688B2/en
Priority to US14/513,507 priority patent/US20150026967A1/en
Abandoned legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • 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
    • 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
    • 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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/381—Alkaline or alkaline earth metals elements
    • 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
    • H01M4/381—Alkaline or alkaline earth metals elements
    • H01M4/382—Lithium
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/49108—Electric battery cell making
    • Y10T29/49115—Electric battery cell making including coating or impregnating

Definitions

  • the invention relates to chemical Protection of a metal surface.
  • Electrochemical cells containing a metallic anode, a cathode and a solid or solvent-containing electrolyte are known in the art. Such batteries have limitations over repeated charge/discharge cycles and may have drops in their charge and discharge capacity over repeated cycles as compared to their initial charge and discharge capacity. Additionally, an initial capacity of solid batteries is often less than desirable. There is therefore a need in the art for an improved battery having a high initial capacity and maintains such a capacity on repeated charge and discharge cycles.
  • Dendrites may be formed on the anode when the electrochemical cell is charged.
  • the dendrite may grow over repeated cycles and lead to a reduced performance of the battery or a short circuit not allowing the charge and discharge of the battery.
  • An electrochemical cell includes an anode having a metal material having an oxygen containing layer.
  • the electrochemical cell also includes a cathode and an electrolyte.
  • the anode includes a chemically bonded protective layer formed by reacting a D or P block precursor with the oxygen containing layer.
  • FIG. 1 is a IR spectroscopy plot of the wavelength versus the intensity for a lithium metal before and after application of the protective layer;
  • FIG. 2 is a differential scanning calorimetry plot for a lithium metal having the protective layer
  • FIG. 3 is a diagram of an experimental setup for impedance testing
  • FIG. 4 is a plot of the impedance for chlorotrimethylsilane precursor forming a protective layer and a reference material
  • FIG. 5 is a plot of the impedance for chlorodiisopropylphosphine precursor forming a protective layer and a reference material
  • FIG. 6 is a plot of the impedance for chlorodiethylphosphine precursor forming a protective layer and a reference material
  • FIG. 7 is a plot of the impedance for dromodimethylborane precursor forming a protective layer and a reference material
  • FIG. 8 is a plot of the resistance for chlorotrimethylsilane, chlorodiisopropylphosphine, chlorodiethylphosphine, dromodimethylborane precursor forming a protective layer and a reference material.
  • electrochemical cell refers to a device having an anode, cathode and an ion-conducting electrolyte interposed between the two.
  • the electrochemical cell may be a battery, capacitor or other such device.
  • the battery may be of a primary or secondary chemistry.
  • the battery may have a solid electrolyte or a liquid electrolyte.
  • anode as used herein refers to an electrode, which oxidizes during a discharge cycle.
  • an electrochemical cell having an anode including a metal material having an oxygen containing layer.
  • the anode metal material may be alkaline metals or alkaline earth metals as indicated in the periodic table.
  • metal materials include: lithium, aluminum, sodium, and magnesium.
  • the metal material is lithium.
  • the oxygen containing layer may be formed by exposing the metal material to the atmosphere or may otherwise be formed on the metal material.
  • the electrochemical cell also includes a cathode, which may be formed of any suitable material.
  • An electrolyte is interposed between the anode and cathode and may be of any suitable form including solid electrolytes liquid electrolytes and gel polymer electrolytes, which are a polymer matrix swollen with solvent and salt. Solid electrolytes could be polymer-type, inorganic layer or mixtures of these two. Examples of polymer electrolytes include, PEO-based, and PEG based polymers.
  • Inorganic electrolytes could be composed of sulfide glasses, phosphide glasses, oxide glasses and mixtures thereof
  • An example of a liquid electrolyte includes carbonate solvent with dissolved metal-ion salt, for example 1M LiPF6 in ethylene carbon/diethyl carbonate (EC/DEC).
  • the anode of the electrochemical cell includes a chemically bonded protective layer formed thereon by reacting a D or P block precursor with the oxygen containing layer.
  • D or P block precursor includes compounds that have elements in the D or P block of the periodic table. Examples of D or P block elements include phosphorus, boron, silicon, titanium, molybdenum, tantalum, vanadium to name a few.
  • the D or P block precursor may be an organo-metallic compound. Examples of organo-metallic compounds include: inter-metaltic compounds, alloys and metals having organic substituents bonded thereon. In a preferred aspect of the invention D or P block precursors may include silicon, boron or phosphorous.
  • the D or P block precursors react with the oxygen containing layer of the metal material to form the protective layer.
  • the D or P block precursor may be a chemical compound of the formula: AR 1 R 2 X wherein A is selected from phosphorous or boron, X is a halogen or halogen containing compound and R 1 is selected from halogens, alkyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, or aromatic groups having from 1 to 20 carbons, R 2 is selected from halogens, alkyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, or aromatic groups having from 1 to 20 carbons.
  • the halogen may be chlorine, bromine, fluorine, and iodine.
  • the alkyl, alkoxy, and aromatic groups may be fluorinated or partially fluorinated.
  • the alcyl group may be methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, tert-pentyl, iso-octyl, tert-octyl, 2-ethyhexyl, nonyl, decyl, undecyl, cyclopentyl, cyclohexyl, cycloheptyl, cyclooctyl, 1-methylcyclopentyl, 1-methylcyclohexyl, 1-methylcyclohexyl, and 1-methyl-4-isopropylcyclohexyl, although other alkyl groups not listed may be used by the invention.
  • the alkyl group may also be functionalized. Suitable functional groups include: ether, sulfide, sulfoxide to name a few.
  • the aromatic group may be phenyl groups, phenyl groups having alkyl substituents in the para, meta or ortho position, and polyaromatic compounds.
  • suitable polyaromatic compounds include naphthalene derivatives.
  • the D or P block precursor may be a chemical compound of the formula: AR 1 R 2 R 3 R 4 X wherein A is phosphorous, X is a halogen or halogen containing compound and R 1 is selected from halogens, alkyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, aromatic groups having from 1 to 20 carbons, or oxygen R 2 is selected from halogens, alkyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, aromatic groups having from 1 to 20 carbons, or oxygen, R3 is selected from halogens, alkyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, aromatic groups having from 1 to 20 carbons, or oxygen, R4 is selected from halogens, alcyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, aromatic groups having from 1 to 20 carbons, or oxygen.
  • A is phosphorous
  • X is a hal
  • the number of R groups may be less than four total.
  • the D or P block precursor may be a chemical compound of the formula: SiR 1 R 2 R 3 X wherein, X is a halogen or halogen containing compound and R 1 is selected from hydrogen, halogens, alkyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, or aromatic groups having from 1 to 20 carbons, R 2 is selected from hydrogen, halogens, alkyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, or aromatic groups having from 1 to 20 carbons R 3 is selected from hydrogen, halogens, alkyl groups having from 1 to 20 carbons, alkoxy groups containing 1 to 20 carbons, or aromatic groups having from 1 to 20 carbons.
  • lithium metal strips were exposed to various precursor compounds.
  • the lithium strips were placed in a sealed flask at room temperature in an inert atmosphere containing the precursor compound.
  • the strips were exposed to the precursor a suitable period of time for the precursor to react with the metal oxygen containing layer on the lithium to form the protective layer.
  • Various analysis procedures were performed including: impedance tests, IR spectroscopy tests, and differential scanning calorimetry tests on the various samples.
  • FIG. 1 An untreated sample of the lithium metal and a sample treated with chlorotrimethyl silane for 240 seconds according to the above procedure were analyzed using IR spectroscopy, as shown in FIG. 1 .
  • the peak correspond to a lithium hydroxide bond is shown in the 3600 cm ⁇ 1 range for the untreated sample. This peak is not shown for the treated sample which includes a peak in the 1100 cm ⁇ 1 range corresponding to a silicon oxygen bond. This relationship indicates the precursor compound has reacted with the metal oxygen containing to form a silicon oxygen bond.
  • An untreated sample of the lithium metal and a sample treated with chlorotrimethyl silane according to the above procedure were analyzed using differential scanning calorimetry, as shown in FIG. 2 .
  • the samples were placed in aluminum pans with nitrogen gas flowing around the samples. The samples were heated to above the melting point and cooled below the melting point repetitively to determine whether the lithium was protected from the environment.
  • the untreated lithium sample reacted with the aluminum pan and did not show melting and solidification representative of pure lithium metal.
  • the treated sample, as shown in FIG. 2 exhibits very clear melting and solidification of lithium at or very near the melting point of lithium (the slight amount of superheating or supercooling at the melting point is heating rate dependent). The narrow peaks indicate that the lithium metal is protected and has not reacted with its environment in contrast to the unprotected sample.
  • FIG. 4 shows the impedance plot for a sample treated with a chlorotrimethylsilane precursor forming a protective layer.
  • FIG. 5 is a plot of the impedance for a chlorodiisopropylphosphine precursor forming a protective layer.
  • FIG. 6 is a plot of the impedance for a chlorodiethylphosphine precursor forming a protective layer.
  • FIG. 7 is a plot of the impedance for a dibromodimethylborane precursor forming a protective layer.
  • the treated samples all have an impedance curve with a slope less than the reference samples. This behavior indicates an improved performance in comparison to the untreated samples.
  • the impedance values were used to calculate a resistance of the various samples, which are displayed in FIG. 8 for the various samples. As can be seen in the figure, the resistance for all the treated samples is less than the untreated reference.
  • the various elements and R groups of the precursor material has an affect on the resistance of the samples.
  • the chlorodiisopropylphosphine sample shows the lowest resistance of the treated samples. A lower resistance metal material is desirable for use as an anode in an electrochemical cell.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Secondary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
US11/457,525 2005-09-02 2006-07-14 Chemical protection of metal surface Abandoned US20070082268A1 (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
US11/457,525 US20070082268A1 (en) 2005-09-02 2006-07-14 Chemical protection of metal surface
CN2007800325285A CN101542782B (zh) 2006-07-14 2007-05-24 金属表面的化学保护
PCT/US2007/012613 WO2008008130A2 (en) 2006-07-14 2007-05-24 Chemical protection of metal surface
KR1020097002913A KR101501565B1 (ko) 2006-07-14 2007-05-24 금속 표면의 화학적 보호
JP2009519433A JP5336363B2 (ja) 2006-07-14 2007-05-24 金属表面の化学的保護
US12/396,223 US20090220857A1 (en) 2005-09-02 2009-03-02 Chemical protection of metal surface
US14/156,241 US20140134488A1 (en) 2006-07-14 2014-01-15 Chemical protection of metal surface
US14/163,536 US8840688B2 (en) 2006-07-14 2014-01-24 Chemical protection of metal surface
US14/513,507 US20150026967A1 (en) 2006-07-14 2014-10-14 Chemical protection of metal surface

Applications Claiming Priority (3)

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US71368805P 2005-09-02 2005-09-02
US73949905P 2005-11-23 2005-11-23
US11/457,525 US20070082268A1 (en) 2005-09-02 2006-07-14 Chemical protection of metal surface

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US12/396,223 Continuation-In-Part US20090220857A1 (en) 2005-09-02 2009-03-02 Chemical protection of metal surface
US14/163,536 Continuation US8840688B2 (en) 2006-07-14 2014-01-24 Chemical protection of metal surface

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US (2) US20070082268A1 (enrdf_load_stackoverflow)
JP (1) JP5336363B2 (enrdf_load_stackoverflow)
KR (1) KR101501565B1 (enrdf_load_stackoverflow)
CN (1) CN101542782B (enrdf_load_stackoverflow)
WO (1) WO2008008130A2 (enrdf_load_stackoverflow)

Cited By (6)

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Publication number Priority date Publication date Assignee Title
US20080069944A1 (en) * 2006-09-19 2008-03-20 Toyota Engineering & Manufacturing North America, Inc. Method of chemical protection of metal surface
US20090220857A1 (en) * 2005-09-02 2009-09-03 Toyota Motor Engineering & Manufacturing North America, Inc. Chemical protection of metal surface
WO2013104788A1 (de) 2012-01-13 2013-07-18 Chemetall Gmbh Phosphorbeschichtete lithiummetallprodukte, verfahren zu deren herstellung und verwendung
DE102013200416A1 (de) 2012-01-13 2013-07-18 Chemetall Gmbh Stabilisierte mit legierungsbildenden Elementen beschichtete Lithiummetallabformungen und Verfahren zu deren Herstellung
WO2014170429A1 (de) 2013-04-19 2014-10-23 Rockwood Lithium GmbH Stabilisierte mit einer stickstoffhaltigen schale beschichtete lithiummetallabformungen und verfahren zu deren herstellung
US20220216462A1 (en) * 2019-05-13 2022-07-07 Korea Electrotechnology Research Institute Anode active material comprising metal phosphide coating on surface of carbon material, preparation method therefor, nonaqueous lithium secondary battery comprising anode active material, and manufacturing method therefor

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US8217930B2 (en) 2009-08-27 2012-07-10 3M Innovative Properties Company Fast transitions of large area cholesteric displays

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CN102405543A (zh) * 2009-03-02 2012-04-04 丰田自动车工程及制造北美公司 金属表面的化学保护
JP2012519368A (ja) * 2009-03-02 2012-08-23 トヨタ モーター エンジニアリング アンド マニュファクチャリング ノース アメリカ，インコーポレイティド 金属表面の化学的保護
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DE102013200416A1 (de) 2012-01-13 2013-07-18 Chemetall Gmbh Stabilisierte mit legierungsbildenden Elementen beschichtete Lithiummetallabformungen und Verfahren zu deren Herstellung
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DE102013200414A1 (de) 2012-01-13 2014-01-09 Chemetall Gmbh Phosphorbeschichtete Lithiummetallprodukte, Verfahren zu deren Herstellung und Verwendung
US9601762B2 (en) 2012-01-13 2017-03-21 Rockwood Lithium GmbH Phosphorous-coated lithium metal products, method for production and use thereof
US11018334B2 (en) 2012-01-13 2021-05-25 Albemarle Germany Gmbh Stabilized lithium metal impressions coated with alloy-forming elements and method for production thereof
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US8840688B2 (en) 2014-09-23
KR20090058504A (ko) 2009-06-09
JP5336363B2 (ja) 2013-11-06
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CN101542782A (zh) 2009-09-23
JP2009544115A (ja) 2009-12-10

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