JP3172388B2 - Lithium secondary battery - Google Patents

Lithium secondary battery

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Publication number
JP3172388B2
JP3172388B2 JP06497595A JP6497595A JP3172388B2 JP 3172388 B2 JP3172388 B2 JP 3172388B2 JP 06497595 A JP06497595 A JP 06497595A JP 6497595 A JP6497595 A JP 6497595A JP 3172388 B2 JP3172388 B2 JP 3172388B2
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positive electrode
lithium
secondary battery
lithium secondary
battery
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JPH08236114A (en
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良浩 小路
俊彦 斎藤
丸男 神野
晃治 西尾
伸道 西田
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三洋電機株式会社
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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
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies or technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage
    • Y02E60/12Battery technologies with an indirect contribution to GHG emissions mitigation
    • Y02E60/122Lithium-ion batteries

Description

【発明の詳細な説明】 DETAILED DESCRIPTION OF THE INVENTION

【0001】 [0001]

【産業上の利用分野】本発明は、リチウム−遷移金属複合酸化物を正極活物質とするリチウム二次電池に係わり、詳しくは充放電サイクル特性を改善することを目的とした、正極の改良に関する。 BACKGROUND OF THE INVENTION The present invention is a lithium - transition metal composite oxide relates to a lithium secondary battery positive electrode active material, specifically aimed to improve the charge-discharge cycle characteristics, an improvement of the positive electrode .

【0002】 [0002]

【従来の技術及び発明が解決しようとする課題】近年、 BACKGROUND OF INVENTION Problems to be Solved In recent years,
リチウム二次電池が、水の分解電圧を考慮する必要がなく、正極活物質を適宜選定することにより高電圧化を達成することが可能であることから、注目されつつある。 Lithium secondary battery, it is not necessary to consider the decomposition voltage of water, since it is possible to achieve a higher voltage by selecting the cathode active material suitably is attracting attention.

【0003】この種の電池の代表的な正極活物質としては、容易に作製することができるとともに、容量が大きいことから、LiV 38 、LiFeO 2 、LiNiO [0003] Representative positive electrode active material of this type of battery, it is possible to easily produce, since capacitance is large, LiV 3 O 8, LiFeO 2 , LiNiO
2 、LiCoO 2 、LiMnO 2 、LiMn 24などのリチウム−遷移金属複合酸化物が主に使用されている。 2, lithium such as LiCoO 2, LiMnO 2, LiMn 2 O 4 - transition metal composite oxide is mainly used.

【0004】しかしながら、リチウム−遷移金属複合酸化物を正極活物質として使用したリチウム二次電池には、充放電サイクル特性が未だ実用上充分満足の行く程度のものではないという問題がある。 However, lithium - the lithium secondary battery using transition metal composite oxide as a cathode active material, there is a problem that the charge-discharge cycle characteristics not yet such a degree that goes practically satisfactory. これは、リチウム−遷移金属複合酸化物を正極活物質とする正極は表面の活性が高いために、正極表面で電解液(非水電解液)が分解することによるものである。 This lithium - positive to the transition metal compound oxide as a positive electrode active material due to the high activity of the surface is by the electrolyte in the positive electrode surface (the non-aqueous electrolyte solution) decomposes.

【0005】本発明は、この問題を解決するべくなされたものであって、その目的とするところは、正極表面での電解液の分解を抑制することにより、充放電サイクル特性に優れたリチウム二次電池を提供するにある。 [0005] The present invention, which solve such problem, it is an object by suppressing the decomposition of the electrolyte at the cathode surface, a lithium secondary excellent charge-discharge cycle characteristics It is to provide the following battery.

【0006】 [0006]

【課題を解決するための手段】上記目的を達成するための本発明に係るリチウム二次電池(本発明電池)は、リチウム−遷移金属複合酸化物を活物質とする正極を備えるリチウム二次電池であって、前記正極の表面に、Be The lithium secondary battery according to the present invention for achieving the above object, according to an aspect of (present battery) is lithium - lithium secondary battery comprising a positive electrode for a transition metal composite oxide as an active material a is the surface of the positive electrode, be
O、MgO、CaO、SrO、BaO、ZnO、Al 2 O, MgO, CaO, SrO, BaO, ZnO, Al 2
3 、CeO 2 、As 23又はこれらの2種以上の混合物からなる被膜が形成されていることを特徴とする。 O 3, wherein the coating film made of CeO 2, As 2 O 3 or a mixture of two or more thereof are formed.

【0007】上記リチウム−遷移金属複合酸化物としては、LiV 38 、LiFeO 2 、LiNiO 2 、Li [0007] The lithium - transition metal composite oxide, LiV 3 O 8, LiFeO 2 , LiNiO 2, Li
CoO 2 、LiMnO 2 、LiMn 24が例示される。 CoO 2, LiMnO 2, LiMn 2 O 4 are exemplified. 充放電サイクル特性に特に優れた電池を得る上で、 In order to obtain a particularly excellent battery charge-discharge cycle characteristics,
一般式Li X Ni 1-y Co yz (但し、0<x<1. Formula Li X Ni 1-y Co y O z ( where, 0 <x <1.
3、0≦y≦1、1.8<z<2.2)で表されるリチウム−遷移金属複合酸化物が特に好ましい。 3,0 ≦ y ≦ 1,1.8 <Lithium represented by z <2.2) - transition metal composite oxide is particularly preferred.

【0008】上記被膜としては、充放電サイクル特性に特に優れた電池を得る上で、BeO、MgO、CaO、 [0008] Examples of the coating, in order to obtain a particularly excellent battery charge-discharge cycle characteristics, BeO, MgO, CaO,
SrO、BaO、ZnO又はこれらの2種以上の混合物からなる被膜が特に好ましい。 SrO, BaO, is film composed of ZnO or a mixture of two or more thereof are particularly preferred.

【0009】上記被膜を形成するための方法としては、 As a method for forming the coating,
CVD(Chemical Vapor Deposition)、蒸着法、スパッタリングが例示される。 CVD (Chemical Vapor Deposition), vapor deposition, sputtering and the like.

【0010】本発明の特徴は、リチウム−遷移金属複合酸化物を活物質とする正極の表面に特定の被膜を形成した点にある。 [0010] Features of the present invention, a lithium - lies in the formation of the specific film on the surface of the positive electrode of a transition metal composite oxide as an active material. それゆえ、負極材料、非水電解液など、電池を構成する他の部材については、従来リチウム二次電池用として提案され、或いは実用されている種々の材料を特に制限なく用いることが可能である。 Therefore, the negative electrode material, a non-aqueous electrolyte solution such as, for other members constituting the battery, is proposed as a conventional lithium secondary battery, or may be used without any particular limitation various materials have been practically used .

【0011】例えば、負極材料としては、リチウムイオンを電気化学的に吸蔵及び放出することが可能な物質又は金属リチウムを使用することができる。 [0011] For example, as the negative electrode material, it is possible to use materials, and metal lithium that is capable of electrochemically occluding and releasing lithium ions. リチウムイオンを電気化学的に吸蔵及び放出することが可能な物質としては、黒鉛、コークス、有機物焼成体等の炭素材料及びリチウム合金(リチウム−アルミニウム合金、リチウム−鉛合金、リチウム−錫合金)が例示される。 Examples of the substance capable of electrochemically occluding and releasing lithium ions include graphite, coke, carbon materials and lithium alloys calcined organic material such as (lithium - aluminum alloy, a lithium - lead alloy, lithium - tin alloy) is It is exemplified.

【0012】また、非水電解液の溶媒としては、エチレンカーボネート、ビニレンカーボネート、プロピレンカーボネートなどの高誘電率溶媒や、これらとジエチルカーボネート、ジメチルカーボネート、1,2−ジメトキシエタン、1,2−ジエトキシエタン、エトキシメトキシエタンなどの低沸点溶媒との混合溶媒が、同溶質としては、LiPF 6 、LiClO 4 、LiCF 3 SO 3 [0012] As the solvent of the nonaqueous electrolyte solution, ethylene carbonate, vinylene carbonate, a high dielectric constant and a solvent, these and diethyl carbonate such as propylene carbonate, dimethyl carbonate, 1,2-dimethoxyethane, 1,2-di ethoxy ethane, a mixed solvent of low boiling point solvent such as ethoxymethoxy ethane, as the same solute, LiPF 6, LiClO 4, LiCF 3 SO 3,
LiN(CF 3 SO 22 、LiBF 4 、LiAsF 6 LiN (CF 3 SO 2) 2 , LiBF 4, LiAsF 6
が、それぞれ例示される。 There are respectively illustrated.

【0013】 [0013]

【作用】正極の表面に特定の金属酸化物からなる被膜が形成されているので、リチウム−遷移金属複合酸化物と電解液との反応が起こりにくくなり、正極の表面での電解液の分解が抑制される。 [Action] Since the film made of a specific metal oxide on the surface of the positive electrode is formed, a lithium - hardly occurs reaction of a transition metal composite oxide and the electrolyte solution, decomposition of the electrolyte at the surface of the positive electrode It is suppressed.

【0014】 [0014]

【実施例】以下、本発明を実施例に基づいてさらに詳細に説明するが、本発明は下記実施例に何ら限定されるものではなく、その要旨を変更しない範囲において適宜変更して実施することが可能なものである。 EXAMPLES The following provides a more detailed explanation of the present invention based on examples, the present invention is not intended to be limited to the following examples, it is carried out appropriately modified within a scope not changing the gist thereof it is those that can be.

【0015】(実施例1〜10) 〔正極〕LiOHとNi(OH) 2 Co(OH) 2とをモル比2:1:1で乳鉢にて混合し、乾燥空気雰囲気下にて750°Cで20時間熱処理し、石川式らいかい乳鉢にて粉砕して、平均粒径5μmのLiNi 0.5 Co [0015] (Examples 1-10) [Positive Electrode LiOH and Ni (OH) 2 Co (OH) 2 and a molar ratio of 2: 1 were mixed in a mortar with 1, 750 ° C under a dry air atmosphere in heat-treated for 20 hours, and pulverized in an Ishikawa automated mortar mortar, having an average particle size of 5 [mu] m LiNi 0.5 Co
0.52を得た。 It was obtained 0.5 O 2.

【0016】次いで、この正極活物質としてのLiNi [0016] Then, LiNi as the positive electrode active material
0.5 Co 0.52と、導電剤としてのアセチレンブラックと、結着剤としてのポリフッ化ビニリデンとを、重量比90:6:4で混合して正極合剤を調製し、この正極合剤を2トン/cm 2の成型圧で直径20mmの円盤状に加圧成型した後、250°Cで2時間熱処理して正極(A)を作製した(実施例1〜9)。 And 0.5 Co 0.5 O 2, acetylene black as a conductive agent, and polyvinylidene fluoride as a binder, the weight ratio of 90: 6 were mixed with 4 a positive electrode mixture was prepared, the positive electrode mixture 2 after compression molding into a disc having a diameter of 20mm at a molding pressure of ton / cm 2, to prepare a positive electrode (a) was heat treated 2 hours at 250 ° C (examples 1-9).

【0017】また、正極活物質としてLiMn 24を使用したこと以外は上記と同様にして、正極(B)を作製した(実施例10)。 Further, except for using LiMn 2 O 4 as the positive electrode active material in the same manner as above, to prepare a positive electrode (B) (Example 10).

【0018】次いで、下記の条件のスパッタリングを行って、上記正極(A)又は(B)の表面に、表1に示す種々の金属酸化物からなる厚さ約1μmの被膜を形成した。 [0018] Then, by performing sputtering under the following conditions, the surface of the positive electrode (A) or (B), to form a thickness of about 1μm of the film consisting of various metal oxides shown in Table 1. なお、被膜の厚み(金属酸化物の担持量)はスパッタリング時間で制御した。 Incidentally, (supported amount of the metal oxide) coating thickness was controlled by the sputtering time.

【0019】(スパッタリングの条件) 真空度:1×10 -7トール(torr) アルゴン(Ar)圧:1×10 -5トール [0019] (sputtering conditions) vacuum: 1 × 10 -7 Torr (torr) argon (Ar) pressure: 1 × 10 -5 Torr

【0020】 [0020]

【表1】 [Table 1]

【0021】〔負極〕所定の厚みの金属リチウム圧延板を直径20mmの円盤状に打ち抜いて負極を作製した。 [0021] A metal lithium rolled plate of [negative] predetermined thickness punched into a disc having a diameter of 20mm to produce a negative electrode.

【0022】〔非水電解液〕エチレンカーボネートとジエチルカーボネートとの体積比1:1の混合溶媒に、六フッ化リン酸リチウムを1M(モル/リットル)溶かして非水電解液を調製した。 [0022] [non-aqueous electrolyte] volume ratio of ethylene carbonate and diethyl carbonate 1: a mixed solvent of 1, lithium hexafluorophosphate was prepared 1M (mol / l) dissolved in non-aqueous electrolyte solution.

【0023】〔電池の組立〕以上の正負極及び非水電解液を用いて扁平形の本発明電池BA1〜BA10を組み立てた(電池寸法:直径24.0mm、厚さ3.0m [0023] assembling the present invention battery BA1~BA10 of flat-shaped with a positive and negative electrode and the nonaqueous electrolyte of the above [Assembly of Battery] (battery size: diameter 24.0 mm, thickness of 3.0m
m)。 m). なお、セパレータとしては、ポリプロピレン製の微多孔膜を使用し、これに先の非水電解液を含浸させた。 As the separator, using a polypropylene microporous film was which is impregnated with non-aqueous electrolyte above.

【0024】図1は、作製した本発明電池を模式的に示す断面図であり、図示の本発明電池Aは、正極(正極(A)又は(B)の表面に特定の金属酸化物からなる被膜を形成したもの。)1、負極2、これら両電極1,2 [0024] Figure 1 is a cross-sectional view schematically showing the present invention battery produced, the present invention cell A illustrated, comprising a specific metal oxide on the surface of the positive electrode (positive electrode (A) or (B) those to form a coating film.) 1, a negative electrode 2, the both electrodes 1, 2
を互いに離間するセパレータ3、正極缶4、負極缶5、 The spaced apart from each other separator 3, positive electrode can 4, a negative electrode can 5,
正極集電体6、負極集電体7及びポリプロピレン製の絶縁パッキング8などからなる。 Positive electrode current collector 6, and the like negative electrode current collector 7 and a polypropylene insulating packing 8.

【0025】正極1及び負極2は、非水電解液を含浸したセパレータ3を介して対向して正負極缶4,5が形成する電池ケース内に収納されており、正極1は正極集電体6を介して正極缶4に、又負極2は負極集電体7を介して負極缶5に接続され、電池内部に生じた化学エネルギーを正極缶4及び負極缶5の両端子から電気エネルギーとして外部へ取り出し得るようになっている。 The positive electrode 1 and negative electrode 2, a non-aqueous electrolyte housed in a battery case positive and negative electrode cans 4 and 5 are formed to face each other with a separator 3 impregnated with the positive electrode 1 is the cathode current collector 6 positive electrode can 4 via, and the negative electrode 2 is connected to the negative electrode can 5 via the negative electrode current collector 7, as electrical energy to chemical energy generated inside the battery from the terminals of the positive electrode can 4 and the negative electrode can 5 so that the can be taken out.

【0026】(比較例1,2)正極の表面に被膜を形成しなかったこと以外は実施例1〜10と同様にして、比較電池BC1,BC2を組み立てた。 [0026] (Comparative Examples 1 and 2) except for not forming a film on the surface of the positive electrode in the same manner as in Examples 1 to 10 were assembled comparative battery BC1, BC2. 但し、比較電池B However, the comparative batteries B
C1は、正極(A)を使用したものであり、比較電池B C1 is obtained by using the positive electrode (A), the comparative battery B
C2は正極(B)を使用したものである。 C2 is obtained by using the positive electrode (B).

【0027】〔充放電サイクル特性〕本発明電池BA1 [0027] Charge-discharge cycle characteristics The present invention battery BA1
〜BA10及び比較電池BC1,2について、電流密度1mA/cm 2で4.3Vまで充電した後、電流密度3 For ~BA10 and Comparative Batteries BC1,2, was charged at a current density of 1 mA / cm 2 up to 4.3 V, the current density 3
mA/cm 2で2.5Vまで放電する工程を1サイクルとする充放電サイクル試験を行い、充放電サイクル特性を調べた。 a step of discharging at mA / cm 2 to 2.5V subjected to the charge-discharge cycle test in which one cycle was examined charge-discharge cycle characteristics. 各電池の1サイクル目の放電容量、400サイクル目の放電容量及び容量維持率〔容量維持率(%) Discharge capacity at the first cycle of each battery, 400 discharge capacity and capacity retention rate cycle [capacity maintenance ratio (%)
=(400サイクル目の放電容量/1サイクル目の放電容量)×100〕を先の表1に示す。 = Indicates a (400th cycle discharge capacity / 1st cycle discharge capacity) × 100] in the previous Table 1.

【0028】表1に示すように、正極表面に特定の被膜を形成した本発明電池BA1〜BA10は、正極表面に被膜を形成しなかった比較電池BC1,BC2に比べて、容量維持率が大きい。 As shown in Table 1, the present invention battery BA1~BA10 forming a specific coating on the positive electrode surface, as compared with the comparison battery BC1, BC2 which did not form a film on the positive electrode surface, a large capacity maintenance ratio . 特に、正極が同じ本発明電池BA1〜BA9のうちBA4〜BA9の容量維持率が特に大きい。 In particular, the capacity retention BA4~BA9 of the positive electrode is the same present batteries BA1~BA9 is particularly large. このことから、被膜形成材料としてはBe Therefore, as the film-forming material Be
O、MgO、CaO、SrO、BaO又はZnOが特に好ましいことが分かる。 O, MgO, CaO, SrO, be BaO or ZnO is particularly preferable seen. また、本発明電池BA9と本発明電池BA10との比較から、正極活物質としては、L Further, from the comparison of the present invention battery BA9 and present battery BA10, as the positive electrode active material, L
iMn 24よりもLiNi 0.5 Co 0.52に代表される式Li X Ni 1-y Co yz (但し、0<x<1. IMN 2 O 4 as represented by LiNi 0.5 Co 0.5 O 2 than formula Li X Ni 1-y Co y O z ( where, 0 <x <1.
3、0≦y≦1、1.8<z<2.2)で表されるリチウム−遷移金属複合酸化物を使用することが好ましいことが分かる。 3,0 ≦ y ≦ 1,1.8 <Lithium represented by z <2.2) - it can be seen it is preferred to use transition metal composite oxide.

【0029】上記実施例では、リチウム−遷移金属複合酸化物としてLiNi 0.5 Co 0.52又はLiMn 2 [0029] In the above embodiment, a lithium - LiNi 0.5 Co 0.5 O 2 or LiMn 2 as the transition metal complex oxide
4を使用したが、本発明は、種々のリチウム−遷移金属複合酸化物を正極活物質とするリチウム二次電池に適用し得るものである。 While using O 4, the present invention provides a variety of lithium - it is capable of applying a transition metal complex oxide in the lithium secondary battery positive electrode active material.

【0030】また、上記実施例では、本発明を扁平形のリチウム二次電池に適用する場合を例に挙げて説明したが、本発明電池の形状に特に制限はない。 Further, in the above embodiment, although the case of applying the present invention to a lithium secondary battery of the flat-shaped has been described as an example, there is no particular limitation on the shape of the present invention the battery.

【0031】 [0031]

【発明の効果】本発明電池は、充電時に正極の表面で非水電解液の分解が起こりにくいので、充放電サイクル特性に優れる。 Present battery according to the present invention, since the decomposition of the nonaqueous electrolyte solution at the surface of the positive electrode is unlikely to occur during charging, and excellent charge-discharge cycle characteristics.

【図面の簡単な説明】 BRIEF DESCRIPTION OF THE DRAWINGS

【図1】実施例で組み立てた扁平形のリチウム二次電池の断面図である。 1 is a cross-sectional view of a lithium secondary battery of flat-shaped assembled in the Examples.

【符号の説明】 DESCRIPTION OF SYMBOLS

1 正極 2 負極 3 セパレータ 1 positive electrode 2 negative electrode 3 separator

───────────────────────────────────────────────────── フロントページの続き (72)発明者 西尾 晃治 大阪府守口市京阪本通2丁目5番5号 三洋電機株式会社内 (72)発明者 斎藤 俊彦 大阪府守口市京阪本通2丁目5番5号 三洋電機株式会社内 (56)参考文献 特開 昭61−7577(JP,A) 特開 平6−150928(JP,A) (58)調査した分野(Int.Cl. 7 ,DB名) H01M 4/02 H01M 10/40 ────────────────────────────────────────────────── ─── of the front page continued (72) inventor Nishio AkiraOsamu Osaka Prefecture Moriguchi Keihanhondori 2-chome No. 5 No. 5, Sanyo Electric Co., Ltd. in the (72) inventor Toshihiko Saito Osaka Prefecture Moriguchi Keihanhondori 2-chome No. 5 No. 5 Sanyo Electric Co., Ltd. in the (56) reference Patent Sho 61-7577 (JP, a) JP flat 6-150928 (JP, a) (58 ) investigated the field (Int.Cl. 7, DB name) H01M 4/02 H01M 10/40

Claims (3)

    (57)【特許請求の範囲】 (57) [the claims]
  1. 【請求項1】リチウム−遷移金属複合酸化物を活物質とする正極を備えるリチウム二次電池において、前記正極の表面に、BeO、MgO、CaO、SrO、BaO、 1. A lithium - in a lithium secondary battery comprising a positive electrode for a transition metal composite oxide as an active material, the surface of the positive electrode, BeO, MgO, CaO, SrO, BaO,
    ZnO、Al 23 、CeO 2 、As 23又はこれらの2種以上の混合物からなる被膜が形成されていることを特徴とするリチウム二次電池。 ZnO, Al 2 O 3, CeO 2, As 2 O 3 or a lithium secondary battery, characterized by the coating consisting of two or more thereof are formed.
  2. 【請求項2】リチウム−遷移金属複合酸化物を活物質とする正極を備えるリチウム二次電池において、前記正極の表面に、BeO、MgO、CaO、SrO、BaO、 2. A lithium - in a lithium secondary battery comprising a positive electrode for a transition metal composite oxide as an active material, the surface of the positive electrode, BeO, MgO, CaO, SrO, BaO,
    ZnO又はこれらの2種以上の混合物からなる被膜が形成されていることを特徴とするリチウム二次電池。 Lithium secondary battery, characterized in that coating of ZnO or a mixture of two or more thereof are formed.
  3. 【請求項3】前記リチウム−遷移金属複合酸化物が、式Li X Ni 1-y Co yz (但し、0<x<1.3、0 Wherein the lithium - transition metal composite oxide has the formula Li X Ni 1-y Co y O z ( where, 0 <x <1.3,0
    ≦y≦1、1.8<z<2.2)で表されるものである請求項1又は2記載のリチウム二次電池。 ≦ y ≦ 1,1.8 <lithium secondary battery according to claim 1 or 2, wherein is represented by z <2.2).
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