JP2006260886A - Porous metal anode and lithium secondary battery using the same - Google Patents

Porous metal anode and lithium secondary battery using the same Download PDF

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JP2006260886A
JP2006260886A JP2005074936A JP2005074936A JP2006260886A JP 2006260886 A JP2006260886 A JP 2006260886A JP 2005074936 A JP2005074936 A JP 2005074936A JP 2005074936 A JP2005074936 A JP 2005074936A JP 2006260886 A JP2006260886 A JP 2006260886A
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lithium
negative electrode
secondary battery
metal
porous
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JP5031193B2 (en
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Akihiko Ban
Kaoru Dotsuko
Kiyoshi Kanemura
明彦 伴
薫 獨古
聖志 金村
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Japan Science & Technology Agency
独立行政法人科学技術振興機構
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/54Manufacturing of lithium-ion, lead-acid or alkaline secondary batteries

Abstract

PROBLEM TO BE SOLVED: To provide a negative electrode having a porous structure of a metal or alloy alloyed with lithium useful as a negative electrode for a lithium secondary battery, and charge / discharge cycle stability and high output performance using such a porous negative electrode A lithium secondary battery excellent in performance is provided.
A lithium porous metal alloyed with lithium for a lithium secondary battery, having a porosity of 10 to 98% and a pore diameter of 0.05 to 100 μm Metal porous negative electrode alloying with lithium for secondary battery.
[Selection] Figure 1

Description

  The present invention relates to a lithium secondary battery, and more particularly to a long-life, high-power lithium secondary battery using a metal porous body as a negative electrode of a lithium secondary battery.

In recent years, portable devices such as mobile phones, laptop computers, and camera-integrated VTRs have formed a large market.
There is a strong demand for a secondary battery having a light weight, a small size, and a high energy density as a power source used in these portable devices. In particular, lithium ion secondary batteries are superior to other secondary batteries in terms of the required characteristics described above, and active research and development are being performed.

  Conventionally, a secondary battery using metallic lithium as a negative electrode has been developed for communication equipment for a period of time for consumer use. However, the negative electrode made of metallic lithium has a serious problem that the safety and battery performance of the battery are impaired due to the formation of dendrites (resin-like crystals) or active granular lithium which are deposited on the negative electrode surface during charging. was there.

  For this reason, measures such as using black materials such as black ship, coke, coal, and petroleum pitch fired products as the negative electrode have been taken.

In the negative electrode material described above, for example, when graphite is used for the negative electrode, lithium is charged and discharged by occlusion between the graphite layers. In this case, since deposition of lithium metal on the negative electrode surface does not occur, an internal short circuit does not occur during the charging of the battery, and a long-life battery that can be repeatedly charged and discharged can be configured.
However, since graphite uses the intercalation of lithium ions into the graphite crystal as the principle of charge / discharge, it cannot be obtained a charge / discharge capacity of 372 mAh / g or more calculated from LiC 6 which is the maximum lithium introduction compound. There are drawbacks.

On the other hand, research into using a metal material alloyed with lithium for the negative electrode has also been conducted.
It has been reported that when a metal material that forms an alloy with lithium is used as a negative electrode material, a capacity larger than the charge / discharge capacity of 372 mAh / g of graphite can be obtained. So far, it has been reported that tin, silicon, and materials containing them form an alloy with lithium and a capacity higher than 372 mAh / g has been obtained, and is attracting attention as a large capacity negative electrode material.
However, these negative electrodes cause a large volume expansion when forming an alloy with lithium, so that the alloy is pulverized by repeating charging and discharging, and the current collection is impaired thereby reducing the capacity. There is. Furthermore, since the volume expansion of the negative electrode accompanying charging increases the internal pressure of the battery, there is a risk that the battery will burst.

In the case where the metal material alloyed with lithium is used as a negative electrode for a lithium ion secondary battery, an electrode that can withstand actual use and a method for manufacturing the electrode are difficult, and the state of completion has not yet been reached.
That is, it can be said that the biggest problem that impedes commercialization is due to volume change when the negative electrode material forms an alloy with lithium. Therefore, the completion of a negative electrode using a metal material that can be alloyed with lithium, which has solved the above problems, is eagerly desired.

A first object of the present invention is to provide a metal porous negative electrode that is alloyed with lithium having a long life and high output for a lithium secondary battery.
In addition, a second object of the present invention is to provide a lithium secondary battery having excellent charge / discharge cycle stability and high output performance using such a metal porous negative electrode.

Briefly describing the present invention, the first invention of the present invention is a metal porous negative electrode alloyed with lithium for a lithium secondary battery, having a porosity of 10 to 98% and a pore size of 0. The present invention relates to a metal porous negative electrode that is alloyed with lithium for a lithium secondary battery, characterized by being 0.05 to 100 μm.
In addition, a second invention of the present invention relates to a lithium secondary battery using a metal porous negative electrode alloyed with lithium.

  The metal porous negative electrode alloyed with lithium of the present invention has a charge / discharge capacity of 372 mAh / g or more of a conventional graphite negative electrode when used in a lithium secondary battery, and is mounted on an electronic device. A high-power lithium secondary battery that can be reduced in size and weight can be provided. In addition, since the metal porous negative electrode alloyed with lithium according to the present invention operates stably even after repeated charge and discharge, a lithium secondary battery using it can realize a long life and high output. Has an excellent effect.

The technical configuration and embodiments of the present invention will be described in detail below.
The technical configuration and embodiments of the present invention will be described below with reference to the drawings and examples, but the present invention is not limited to these.

As described above, the negative electrode of the lithium secondary battery undergoes a large volume change when the lithium and the material constituting the negative electrode form an alloy in the charge / discharge cycle, which realizes and commercializes a high-performance lithium secondary battery. Is blocking.
The present inventors show that the large volume change (volume expansion) occurring on the negative electrode side of the lithium secondary electrode is effectively absorbed and relaxed by the porous structure shown in FIG. 1 as shown in FIG. For the first time. This is the basis of the present invention.

The present invention comprises a negative electrode for a lithium secondary battery based on the above knowledge, and the metal porous negative electrode alloyed with lithium according to the present invention is a novel negative electrode for a lithium secondary battery. .
Today, as a porous negative electrode material, a carbon material-based material is known. Compared with this, the material of the present invention exhibits a large charge / discharge capacity, and also has a high charge / discharge cycle stability. Shows performance.

  In order to contribute to an understanding of the present invention, first, a method for producing a metal porous negative electrode alloyed with lithium will be described.

The metallic porous negative electrode (hereinafter sometimes simply referred to as a metallic porous negative electrode) that is alloyed with lithium according to the present invention may be produced by a plating technique or the like.
Polymer particles such as polystyrene and PMMA are deposited on a conductive substrate, a metal alloying with lithium is plated on it, and then the polymer particles are removed to remove the polymer particles. Can be produced.
Any known material can be used as the conductive substrate as long as it is a material having electronic conductivity, but a material that does not form an alloy with lithium is particularly preferable. Examples of such a material include copper, nickel, and stainless steel, and copper is preferably used. As the shape of the conductive substrate, a plate shape or a foil shape is practical.

  The polymer particles may be 0.05 to 100 μm, for example. The pore diameter of the resulting porous body (porous body) can be controlled by the particle diameter of the polymer particles used.

  Electrophoresis can be used as a method for depositing the polymer particles on the conductive substrate. It can also be deposited by drying a suspension of particles on a conductive substrate. The thickness for depositing the particles is, for example, 300 microns or less, and preferably adjusted to about 50 to 100 microns. Further, it is preferable that the particles have a close-packed structure on the conductive substrate.

  After the polymer particles are deposited on the conductive substrate as described above, the particles of the polymer particles may be fused by performing a heat treatment at about 80 to 120 ° C. By performing this heat treatment, the particles are fixed when the substrate is immersed in the plating bath and in the plating. When the particles have a regular array structure on the conductive substrate, the finally obtained porous structure also has a regular array structure.

After the polymer particles are deposited on the conductive substrate as described above, a metal alloying with lithium is applied by plating or the like. In the case of plating, a known plating bath can be used for the plating bath. As the metal to be plated, a metal that can be alloyed with lithium in an electrolyte containing lithium ions and an alloy thereof are preferably used. In the present invention, it should be noted that the metal alloying with lithium includes an alloy as described above.
As a metal or alloy to be alloyed with this kind of lithium, a desired metal may be used. For example, in the case of plating, tin or an alloy containing tin, lead, silver, etc. Tin alloys such as Sn-Ni are practical. In the case of a tin alloy, the tin content may be within a range of 5 wt% to 99.995 wt%, for example.

After applying the metal for alloying lithium as described above by, for example, plating, the polymer particles are dissolved and removed by immersing the sample piece in an organic solvent such as toluene, acetone, or tetrahydrofuran. In this way, a porous metal layer such as Sn or Sn alloy having a porous structure can be formed on the conductive substrate.
In the present invention, as a metal porous negative electrode alloyed with lithium, a porous negative electrode having a porosity of 10 to 98% and a pore diameter of 0.05 to 100 μm may be produced by the production method. The porosity may be set as desired in consideration of the mechanical strength of the metal porous electrode, and may be set, for example, at 50 to 80%. Further, the pore diameter may be set as desired in consideration of absorption and relaxation ability of volume change due to alloying with lithium, for example, 0.05 to 5 μm.
The porous structure of the metal porous negative electrode has a structure as shown in FIG.

Next, a method for producing a lithium secondary battery using the metal porous negative electrode of the present invention will be described.
In the present invention, a lithium secondary battery may be configured by directly using the metal porous negative electrode, for example, a Sn negative electrode made of an Sn alloy. Moreover, you may cut | disconnect and use a negative electrode to a desired magnitude | size according to the magnitude | size of a battery.

A lithium secondary battery comprising a combination of the above-described Sn alloy porous negative electrode plate and an electrolyte solution, positive electrode plate, and other battery constituent elements such as a separator, gasket, current collector, sealing plate, cell case, etc. Configure.
The shape of the battery that can be produced is not particularly limited, such as a cylindrical shape, a square shape, or a coin shape. Basically, a negative electrode plate is placed on the cell floor plate, and an electrolyte and a separator are further formed thereon. The positive electrode is placed so as to face the electrode, and it is caulked together with the gasket and the sealing plate to form a secondary battery.

  Non-aqueous solvents that can be used for the electrolyte include propylene carbonate, ethylene carbonate, diethyl carbonate, dimethyl carbonate, ethyl methyl carbonate, 1,2-dimethoxyethane, γ-ptyrolactone, tetrahydrofuran, 2-methyltetrahydrofuran, sulfolane, 1,3 A single organic solvent such as dioxolane or a mixture of two or more organic solvents can be used.

An electrolyte such as LiClO 4 , LiPF 6 , LiBF 4 , LiCF 3 SO 3 , LiA 3 F 3 or the like of about 0.5 to 2.0 M may be dissolved in these solvents.

  In the present invention, a polymer solid electrolyte that is a conductor of an alkali metal cation such as lithium ion can also be used as the electrolyte.

The material of the positive electrode body is not particularly limited, but a metal chalcogen compound that can occlude and release alkali metal cations such as lithium ions during charge and discharge is preferable.
Examples of the metal chalcogen compound include vanadium oxide, vanadium sulfide, molybdenum oxide, molybdenum sulfide, manganese oxide, chromium oxide, titanium oxide, titanium sulfide, and the like. Examples include composite oxides and composite sulfides. Preferably, Cr 3 O 8 , V 2 O 5 , V 5 O 18 , VO 2 , Cr 2 O 5 , MnO 2 , TiO 2 , MoV 2 O 8 , TiS 2 V 2 S 5 MoS 2 , MoS 3 VS 2 Cr 0.25 V 0.75 S 2 , Cr 0.5 V 0.5 S 2, etc.
In addition, LiMY 2 (M is a transition metal such as Co and Ni, Y is a chalcogen compound such as O and S), LiM 2 Y 4 (M is Mn and Y is O), an oxide such as WO 3 , CuS, Sulfides such as Fe 0.25 V 0.75 S 2 and Na 0.1 CrS 2 , phosphorus such as NiPS 8 and FePS 8 , sulfur compounds, selenium compounds such as VSe 2 and NbSe 3, and the like can also be used.
The positive electrode material described above may be mixed with a binder and applied onto a current collector to form a positive electrode plate.

  The separator that holds the electrolytic solution may be made of a material that is generally excellent in liquid retention. For example, a polyolefin resin nonwoven fabric or a porous film may be used. These functions can be expressed by impregnating the electrolytic solution.

  Next, the present invention will be described in more detail with reference to examples. However, the examples are for explaining the present invention in detail, and it is needless to say that the present invention is not limited by these examples. . The “parts” described below are all parts by weight.

(1). Preparation of Tin-Nickel Alloy Porous Negative Electrode A suspension of polystyrene monodispersed spherical particles (diameter 1 μm) dispersed in ethanol was prepared. Using this, polystyrene particles were deposited on a Cu substrate by electrophoresis.
As electrophoresis conditions, a Ni plate was used as the counter electrode, the distance between the electrodes was 1 cm, the applied voltage was 5 V, and the migration time was 10 minutes.
After electrophoresis, the polystyrene on the Cu substrate was dried, and the sample on which the polystyrene particles were deposited was plated using a tin-nickel alloy plating bath.
As the composition of the plating bath, one containing Sn 2+ ions was used. That is, nickel chloride, tin chloride, glycine, potassium pyrophosphate, aqueous ammonia respectively 0.075molL -1, 0.175molL -1, 0.125molL -1 , 0.5molL -1, to a concentration of 5MlL -1 What was dissolved in distilled water was used. As the plating conditions, the cathode current density was set to 360 μA / cm 2 and the bath temperature of the plating bath was set to 50 ° C. After plating, the polystyrene particles were eluted with toluene.

The composition of the tin-nickel alloy porous body obtained as described above was Ni 73 Sn 27 , the area was 1 cm 2 , the thickness was 3 μm, and the weight was 650 μg.
Moreover, the electron micrograph of the porous body obtained as mentioned above is shown in FIG. As shown in FIG. 3, it can be seen that a large number of uniform holes of 1 μm are formed and communication holes are formed.

(2). Performance Evaluation of Tin-Nickel Alloy Porous Negative Electrode The lithium ion charge / discharge performance of the electrode (negative electrode) obtained as described above was evaluated based on the two-electrode electrochemical measurement.
As the electrolyte containing lithium ions, a solution in which LiCiO 4 was dissolved at a rate of 1 mol / L in a solvent in which ethylene carbonate and dimethyl carbonate were mixed at a volume ratio of 1: 1 was used.
The measurement was performed at 1 atm in a glove box under an argon atmosphere using a glass cell.

The results of a charge / discharge test with a current density of 0.05 mA / cm 2 are shown in FIG. A voltage flat portion is observed at a voltage of 1 V or less. It can be seen from the charge / discharge curve of FIG. 4 that the charge / discharge capacity is about 450 mAh / g. This charge / discharge capacity is larger than the theoretical charge / discharge capacity of 372 mAh / g of graphite, indicating that the negative electrode of the present invention is superior. In addition, the negative electrode of the present invention does not show a significant decrease in capacity even after repeated charging and discharging, and is excellent in stability and durability.

  The electron micrograph of the negative electrode after charging / discharging is shown in FIG. A porous structure was observed even after charge and discharge. This means that the porous structure effectively absorbs and relaxes the expansion of the volume of the negative electrode accompanying charge / discharge.

It is a figure explaining the porous structure of a metal porous negative electrode. It is a figure explaining that a porous structure can absorb and relieve the volume expansion when a metallic porous negative electrode is alloyed with lithium. It is an electron micrograph of the tin-nickel alloy type porous negative electrode of the present invention. It is a figure which shows the charging / discharging measurement result of the tin-nickel alloy type porous negative electrode of this invention. It is an electron micrograph after the charge-discharge measurement of the tin-nickel alloy type porous negative electrode of the present invention.

Claims (4)

  1. A metallic porous negative electrode that is alloyed with lithium for a lithium secondary battery, wherein the porosity is 10 to 98%, and the pore diameter is 0.05 to 100 μm. Metal porous negative electrode alloying with lithium.
  2. The metal-made porous negative electrode to be alloyed with lithium according to claim 1, wherein the metal to be alloyed with lithium is tin or a tin alloy.
  3. The metallic porous negative electrode which is alloyed with lithium according to any one of claims 1 to 2, wherein the metallic porous negative electrode which is alloyed with lithium is produced by plating on a conductive substrate. .
  4. The lithium secondary battery which uses the metal porous negative electrode which alloys with lithium of any one of Claims 1-3.

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KR100949332B1 (en) * 2007-08-24 2010-03-26 삼성에스디아이 주식회사 Electrode for rechargeable lithium battery and rechargeable lithium battery including same
DE102010018458A1 (en) 2009-04-28 2011-02-17 Denso Corporation, Kariya-City Non-aqueous electrolyte solution battery negative electrode and non-aqueous electrolyte solution battery with same
KR101097244B1 (en) 2009-09-02 2011-12-21 삼성에스디아이 주식회사 Negative electrode for lithium battery and lithium battery comprising the same
JP2012082125A (en) * 2010-09-17 2012-04-26 Furukawa Electric Co Ltd:The Porous silicon particle and method for manufacturing the same
US20120148918A1 (en) * 2010-10-19 2012-06-14 Yo-Han Kwon Anode of cable-type secondary battery and manufacturing method thereof
JP2012132083A (en) * 2010-12-24 2012-07-12 Sumitomo Electric Ind Ltd Metallic porous body having high corrosion resistance, and method for manufacturing therefor
JP2012164640A (en) * 2011-01-20 2012-08-30 Mitsubishi Materials Corp Negative electrode active material for lithium ion secondary battery, lithium ion secondary battery comprising the negative electrode active material, and method for manufacturing negative electrode active material for lithium ion secondary battery
JP2012164641A (en) * 2011-01-20 2012-08-30 Mitsubishi Materials Corp Negative electrode active material for lithium ion secondary battery, lithium ion secondary battery comprising the negative electrode active material, and method for manufacturing negative electrode active material for lithium ion secondary battery
DE112011102465T5 (en) 2010-07-23 2013-05-08 Tokyo Metropolitan University Porous electrode for a secondary battery
JP2013534698A (en) * 2010-06-28 2013-09-05 エルジー・ケム・リミテッド Negative electrode for cable-type secondary battery and cable-type secondary battery having the same
WO2013161733A1 (en) * 2012-04-24 2013-10-31 昭和電工株式会社 Negative electrode active material for a lithium secondary battery and method for manufacturing same
JP2014017259A (en) * 2013-09-24 2014-01-30 Tokyo Metropolitan Univ Method of manufacturing negative electrode for nonaqueous electrolyte secondary battery
JP2014123575A (en) * 2010-09-03 2014-07-03 Nexeon Ltd Porous electroactive material
US8980428B2 (en) 2010-09-17 2015-03-17 Furukawa Electric Co., Ltd. Porous silicon particles and complex porous silicon particles, and method for producing both
KR101506451B1 (en) 2012-04-16 2015-03-30 주식회사 엘지화학 Anode for Secondary Battery
JP2018517285A (en) * 2015-04-09 2018-06-28 コーチョアン リン Electrode material and energy storage device
US10164262B2 (en) 2010-12-08 2018-12-25 Sumitomo Electric Industries, Ltd. Method for producing a porous metal body

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DE102010018458A1 (en) 2009-04-28 2011-02-17 Denso Corporation, Kariya-City Non-aqueous electrolyte solution battery negative electrode and non-aqueous electrolyte solution battery with same
US8778541B2 (en) 2009-04-28 2014-07-15 Denso Corporation Negative electrode for nonaqueous electrolyte solution battery and nonaqueous electrolyte solution battery having the same
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KR101097244B1 (en) 2009-09-02 2011-12-21 삼성에스디아이 주식회사 Negative electrode for lithium battery and lithium battery comprising the same
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CN103155230A (en) * 2010-07-23 2013-06-12 东京应化工业株式会社 Secondary battery porous electrode
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JP2014123575A (en) * 2010-09-03 2014-07-03 Nexeon Ltd Porous electroactive material
JP2012082125A (en) * 2010-09-17 2012-04-26 Furukawa Electric Co Ltd:The Porous silicon particle and method for manufacturing the same
US8980428B2 (en) 2010-09-17 2015-03-17 Furukawa Electric Co., Ltd. Porous silicon particles and complex porous silicon particles, and method for producing both
US20120148918A1 (en) * 2010-10-19 2012-06-14 Yo-Han Kwon Anode of cable-type secondary battery and manufacturing method thereof
CN103181002B (en) * 2010-10-19 2016-07-13 株式会社Lg化学 The negative pole of cable Type Rechargeable Battery and manufacture method thereof
US9673485B2 (en) * 2010-10-19 2017-06-06 Lg Chem, Ltd. Anode of cable-type secondary battery and manufacturing method thereof
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US10164262B2 (en) 2010-12-08 2018-12-25 Sumitomo Electric Industries, Ltd. Method for producing a porous metal body
JP2012132083A (en) * 2010-12-24 2012-07-12 Sumitomo Electric Ind Ltd Metallic porous body having high corrosion resistance, and method for manufacturing therefor
JP2012164641A (en) * 2011-01-20 2012-08-30 Mitsubishi Materials Corp Negative electrode active material for lithium ion secondary battery, lithium ion secondary battery comprising the negative electrode active material, and method for manufacturing negative electrode active material for lithium ion secondary battery
JP2012164640A (en) * 2011-01-20 2012-08-30 Mitsubishi Materials Corp Negative electrode active material for lithium ion secondary battery, lithium ion secondary battery comprising the negative electrode active material, and method for manufacturing negative electrode active material for lithium ion secondary battery
KR101506451B1 (en) 2012-04-16 2015-03-30 주식회사 엘지화학 Anode for Secondary Battery
WO2013161733A1 (en) * 2012-04-24 2013-10-31 昭和電工株式会社 Negative electrode active material for a lithium secondary battery and method for manufacturing same
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