JP4049571B2 - Nonaqueous electrolyte secondary battery - Google Patents
Nonaqueous electrolyte secondary battery Download PDFInfo
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- JP4049571B2 JP4049571B2 JP2001336620A JP2001336620A JP4049571B2 JP 4049571 B2 JP4049571 B2 JP 4049571B2 JP 2001336620 A JP2001336620 A JP 2001336620A JP 2001336620 A JP2001336620 A JP 2001336620A JP 4049571 B2 JP4049571 B2 JP 4049571B2
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Description
【０００１】
【発明の属する技術分野】
この発明は、正極と負極と非水電解質とを備えた非水電解質二次電池に係り、特に、正極に用いる材料を改善し、過放電になるのを容易に制御できるようにした点に特徴を有するものである。
【０００２】
【従来の技術】
近年、高出力，高エネルギー密度の新型電池の１つとして、非水電解質を用いて、リチウムの酸化，還元を利用した高起電力の非水電解質二次電池が利用されるようになった。
【０００３】
ここで、このような非水電解質二次電池においては、その正極の材料として、リチウムイオンの吸蔵，放出が可能なリチウム・遷移金属複合酸化物が用いられており、一般には、リチウム・コバルト複合酸化物のＬｉＣｏＯ2 等が広く利用されている。
【０００４】
しかし、リチウム・コバルト複合酸化物の原料となるコバルトは資源の埋蔵量が少なく、高価であるため、正極の材料として、他のリチウム・遷移金属複合酸化物を使用することが要望され、このようなリチウム・遷移金属複合酸化物として、安価でかつ資源の埋蔵量の豊富な材料であるマンガンを用いたリチウム・マンガン複合酸化物が検討されるようになった。
【０００５】
しかし、このようなリチウム・マンガン複合酸化物を非水電解質二次電池における正極の材料に使用した場合、この非水電解質二次電池において充放電を繰り返して行うと、リチウム・マンガン複合酸化物からマンガンが溶出して次第に容量が低下し、充放電サイクル特性が悪いという問題があった。
【０００６】
このため、近年においては、特許第３０２４６３６号公報に示されるように、非水電解質二次電池における正極の材料に、リチウム・マンガン複合酸化物とリチウム・ニッケル複合酸化物とを混合させたものを用い、充放電によってリチウム・マンガン複合酸化物からマンガンが溶出するのを抑制して、充放電サイクル特性を向上させることが提案されている。
【０００７】
しかし、上記のように正極の材料に、リチウム・マンガン複合酸化物とリチウム・ニッケル複合酸化物とを混合させたものを用いた場合、放電末期において正極の電位が急激に低下し、十分な容量を有する非水電解質二次電池を得るために放電深度を深くすると、過放電になりやすく、これにより非水電解質二次電池が劣化して容量が著しく低下し、充放電サイクル特性が著しく低下するという問題があった。
【０００８】
【発明が解決しようとする課題】
この発明は、正極と負極と非水電解質とを備えた非水電解質二次電池における上記のような様々な問題を解決することを課題とするものであり、特に、正極の材料にリチウム・マンガン複合酸化物とリチウム・ニッケル複合酸化物とを用いた場合において、放電末期における正極の電位が急激に低下するのを抑制し、十分な容量を有する非水電解質二次電池を得るために放電深度を深くした場合においても、過放電による容量低下を容易に制御することができると共に、充放電サイクル特性にも優れた非水電解質二次電池が得られるようにすることを課題とするものである。
【０００９】
【課題を解決するための手段】
この発明においては、上記のような課題を解決するため、正極と負極と非水電解質とを備えた非水電解質二次電池において、上記の正極の材料に、リチウム・マンガン複合酸化物とリチウム・ニッケル複合酸化物とを混合焼結させた焼結材料を用いるようにしたのである。
【００１０】
そして、この発明における非水電解質二次電池のように、正極の材料に、リチウム・マンガン複合酸化物とリチウム・ニッケル複合酸化物とを混合焼結させた焼結材料を用いると、リチウム・マンガン複合酸化物とリチウム・ニッケル複合酸化物とを単に混合させただけのものを用いる場合に比べて、放電末期における正極の電位の低下が緩やかになり、放電深度を深くした場合においても、過放電による容量低下を容易に制御することができ、充放電サイクル特性に優れた非水電解質二次電池が得られるようになる。
【００１１】
ここで、正極の材料に用いる上記のリチウム・ニッケル複合酸化物としては、例えば、組成式Ｌｉa Ｎｉx Ｍ1-x Ｏ2 （但し、Ｍは、Ｂ，Ｍｇ，Ａｌ，Ｔｉ，Ｍｎ，Ｖ，Ｆｅ，Ｃｏ，Ｃｕ，Ｚｎ，Ｇａ，Ｙ，Ｚｒ，Ｎｂ，Ｍｏ，Ｉｎから選択される１種以上の遷移元素であり、１≦ａ≦１．５，０＜ｘ≦１を満たす。）で表されるものを使用することができ、特に、組成式Ｌｉa Ｎｉx Ｃｏy Ｍｎz Ｏ2 （但し、１≦ａ≦１．５，０＜ｘ≦１，０≦ｙ＜１，０≦ｚ＜１，ｘ＋ｙ＋ｚ＝１を満たす。）で表されるものを使用することが好ましい。
【００１２】
また、正極の材料に用いる上記のリチウム・マンガン複合酸化物としては、例えば、組成式Ｌｉ1+b Ｍｎc Ｍ’d Ｏ4 （但し、Ｍ’は、Ｍｇ，Ａｌ，Ｔｉ，Ｆｅ，Ｃｒからなる群から選択される１種以上の元素であり、０≦ｂ≦１，１≦ｃ≦２，０≦ｄ＜１を満たす。）で表されるスピネル構造のリチウム・マンガン複合酸化物を使用することができ、特に、組成式Ｌｉ1+b Ｍｎc Ｍ’dＯ4 （但し、０≦ｂ≦０．５，１≦ｃ≦２，０≦ｄ＜１を満たす。）で表されるスピネル構造のリチウム・マンガン複合酸化物を使用することが好ましい。
【００１３】
また、上記のリチウム・ニッケル複合酸化物とリチウム・マンガン複合酸化物とを混合させるにあたっては、リチウム・ニッケル複合酸化物とリチウム・マンガン複合酸化物との重量比を１：９〜９：１の範囲にすることが好ましく、より好ましくは、６：４になるようにする。
【００１４】
また、このようにリチウム・ニッケル複合酸化物とリチウム・マンガン複合酸化物とを混合させて焼結させるにあたり、焼成温度が低いと、リチウム・ニッケル複合酸化物とリチウム・マンガン複合酸化物とが十分に焼結されない一方、焼成温度が高くなり過ぎると、リチウム・ニッケル複合酸化物やリチウム・マンガン複合酸化物における酸素が脱離して劣化するため、焼成温度を２００〜９００℃、好ましくは４００〜６００℃にして焼結させるようにする。
【００１５】
【実施例】
以下、この発明に係る非水電解質二次電池について、実施例を挙げて具体的に説明すると共に、この実施例における非水電解質二次電池の場合、放電末期において正極の電位が急激に低下するのが抑制されることを、比較例を挙げて明らかにする。なお、この発明における非水電解質二次電池は、下記の実施例に示したものに限定されず、その要旨を変更しない範囲において適宜変更して実施できるものである。
【００１６】
（実施例１）
実施例１においては、正極を作製するにあたって、ＬｉＮｉ0.4 Ｃｏ0.3 Ｍｎ0.3 Ｏ2 とＬｉ1.1 Ｍｎ1.9 Ｏ4 とを６：４の重量比でらいかい混合させ、これをペレット状に成形した後、５００℃の大気雰囲気中で焼成してＬｉＮｉ0.4 Ｃｏ0.3 Ｍｎ0.3 Ｏ2 とＬｉ1.1 Ｍｎ1.9 Ｏ4 とが混合焼結された焼結材料を得た。
【００１７】
そして、この焼結材料と導電剤の人造黒鉛とを９：１の重量比で混合させて正極合剤を得た。
【００１８】
次いで、この正極合剤と結着剤のポリフッ化ビニリデンとが９５：５の重量比になるようにして、この正極合剤にポリフッ化ビニリデンが５重量％のＮ−メチル−２−ピロリドン溶液を加え、これを混練してスラリーを調製し、このスラリーを厚み２０μｍのアルミニウム箔の両面にドクターブレード法により塗布し、これを１５０℃で２時間真空乾燥させて正極を作製した。
【００１９】
（比較例１）
比較例１においては、正極を作製するにあたって、上記の実施例１の場合と同様に、ＬｉＮｉ0.4 Ｃｏ0.3 Ｍｎ0.3 Ｏ2 とＬｉ1.1 Ｍｎ1.9 Ｏ4 とを６：４の重量比でらいかい混合させる一方、これを焼成させないで使用し、その後は、上記の実施例１の場合と同様にして正極を作製した。
【００２０】
そして、図１に示すように、上記の実施例１及び比較例１において作製した各正極を作用極１１に用いる一方、負極となる対極１２と参照極１３とにそれぞれ金属リチウムを用い、また非水電解液１４としては、エチレンカーボネートとジエチルカーボネートとを１：１の体積比で混合させた混合溶媒にヘキサフルオロリン酸リチウムＬｉＰＦ6 を１ｍｏｌ／ｌの割合で溶解させたものを使用して、実施例１及び比較例１の各試験用電池を作製した。
【００２１】
そして、上記の各正極を作用極１１に使用した実施例１及び比較例１の各試験用電池において、充電電流０．７５ｍＡ／ｃｍ2 で充電終止電圧が４．３Ｖになるまで充電させた後、充電電流０．２５ｍＡ／ｃｍ2 で充電終止電圧が４．３Ｖになるまで充電させた。その後、実施例１及び比較例１の各試験用電池を放電電流０．７５ｍＡ／ｃｍ2 で放電終止電圧が３．１Ｖになるまで放電させ、放電時における参照極１３に対する各正極１１の電位と、放電深度（％）との関係を調べ、実施例１の試験用電池における結果を実線で、比較例１の試験用電池における結果を破線で図２に示した。
【００２２】
この結果、実施例１の試験用電池においては、放電深度が１００％に近づいた時点における正極の電位の低下が、比較例１の試験用電池に比べて緩やかになっており、実施例１の試験用電池の場合、比較例１の試験用電池に比べて、過放電になるのを容易に抑制することができた。
【００２３】
【発明の効果】
以上詳述したように、この発明における非水電解質二次電池においては、その正極の材料に、リチウム・マンガン複合酸化物とリチウム・ニッケル複合酸化物とを混合焼結させた焼結材料を用いるようにしたため、リチウム・マンガン複合酸化物とリチウム・ニッケル複合酸化物とを単に混合させただけのものを用いた場合に比べて、放電末期における正極の電位の低下が緩やかになった。
【００２４】
この結果、この発明における非水電解質二次電池においては、放電深度を深くした場合においても、過放電による容量低下を容易に制御することができ、充放電サイクル特性に優れた非水電解質二次電池が得られるようになった。
【図面の簡単な説明】
【図１】この発明の実施例１及び比較例１において作製した試験用電池の概略説明図である。
【図２】上記の実施例１及び比較例１の試験用電池の放電時における正極の電位と放電深度（％）との関係を示した図である。
【符号の説明】
１１ 作用極（正極）
１２ 対極（負極）
１３ 参照極
１４ 非水電解液[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a non-aqueous electrolyte secondary battery including a positive electrode, a negative electrode, and a non-aqueous electrolyte, and is particularly characterized in that the material used for the positive electrode is improved and overdischarge can be easily controlled. It is what has.
[0002]
[Prior art]
In recent years, as one of new batteries with high output and high energy density, non-aqueous electrolyte secondary batteries using a non-aqueous electrolyte and utilizing oxidation and reduction of lithium have come to be used.
[0003]
Here, in such a non-aqueous electrolyte secondary battery, a lithium / transition metal composite oxide capable of occluding and releasing lithium ions is used as a material for the positive electrode. An oxide such as LiCoO 2 is widely used.
[0004]
However, since cobalt, which is a raw material for lithium-cobalt composite oxide, has a small reserve of resources and is expensive, it is desired to use another lithium-transition metal composite oxide as the positive electrode material. As lithium-transition metal composite oxides, lithium-manganese composite oxides using manganese, which is an inexpensive and resource-rich material, have been studied.
[0005]
However, when such a lithium-manganese composite oxide is used as a positive electrode material in a non-aqueous electrolyte secondary battery, repeated charging / discharging in this non-aqueous electrolyte secondary battery will result in a lithium-manganese composite oxide. There was a problem that the capacity was gradually reduced due to elution of manganese and the charge / discharge cycle characteristics were poor.
[0006]
For this reason, in recent years, as shown in Japanese Patent No. 3024636, a material obtained by mixing a lithium / manganese composite oxide and a lithium / nickel composite oxide with a positive electrode material in a non-aqueous electrolyte secondary battery. It has been proposed to improve the charge / discharge cycle characteristics by suppressing the dissolution of manganese from the lithium / manganese composite oxide by charge / discharge.
[0007]
However, when the material of the positive electrode mixed with lithium / manganese composite oxide and lithium / nickel composite oxide is used as described above, the potential of the positive electrode rapidly decreases at the end of discharge, and sufficient capacity is obtained. If the depth of discharge is increased in order to obtain a nonaqueous electrolyte secondary battery having a non-aqueous electrolyte, overdischarge tends to occur, which causes the nonaqueous electrolyte secondary battery to deteriorate and significantly reduce its capacity, resulting in a marked decrease in charge / discharge cycle characteristics. There was a problem.
[0008]
[Problems to be solved by the invention]
An object of the present invention is to solve the above various problems in a non-aqueous electrolyte secondary battery comprising a positive electrode, a negative electrode, and a non-aqueous electrolyte. When using a composite oxide and a lithium / nickel composite oxide, the depth of discharge is reduced in order to suppress a rapid decrease in the potential of the positive electrode at the end of discharge and to obtain a nonaqueous electrolyte secondary battery having sufficient capacity. It is an object of the present invention to provide a non-aqueous electrolyte secondary battery that can easily control capacity reduction due to overdischarge and has excellent charge / discharge cycle characteristics even when the depth is increased. .
[0009]
[Means for Solving the Problems]
In the present invention, in order to solve the above-described problems, in a non-aqueous electrolyte secondary battery including a positive electrode, a negative electrode, and a non-aqueous electrolyte, the positive electrode material includes lithium-manganese composite oxide and lithium- A sintered material obtained by mixing and sintering a nickel composite oxide was used.
[0010]
When a sintered material obtained by mixing and sintering lithium / manganese composite oxide and lithium / nickel composite oxide is used as the positive electrode material as in the non-aqueous electrolyte secondary battery according to the present invention, lithium / manganese Compared to the case where a composite oxide and a lithium-nickel composite oxide are simply mixed, the potential of the positive electrode gradually decreases at the end of discharge, and overdischarge occurs even when the discharge depth is increased. Therefore, a non-aqueous electrolyte secondary battery with excellent charge / discharge cycle characteristics can be obtained.
[0011]
Here, examples of the lithium-nickel composite oxide used for the positive electrode material include a composition formula Li a Ni x M 1-x O 2 (where M is B, Mg, Al, Ti, Mn, V , Fe, Co, Cu, Zn, Ga, Y, Zr, Nb, Mo, In, and one or more transition elements, satisfying 1 ≦ a ≦ 1.5 and 0 <x ≦ 1. In particular, the composition formula Li a Ni x Co y Mn z O 2 (where 1 ≦ a ≦ 1.5, 0 <x ≦ 1, 0 ≦ y <1,0 ≦ z <1, x + y + z = 1 is preferably satisfied).
[0012]
Furthermore, as the lithium-manganese composite oxide used in the material of the positive electrode, for example, the composition formula Li 1 + b Mn c M ' d O 4 ( where, M' is, Mg, Al, Ti, Fe, Cr, at least one element selected from the group consisting, using 0 ≦ b ≦ 1,1 ≦ c ≦ 2, 0 ≦ d < satisfies 1.) of lithium-manganese composite oxide having a spinel structure represented by In particular, it is represented by the composition formula Li 1 + b Mn c M ′ d O 4 (where 0 ≦ b ≦ 0.5, 1 ≦ c ≦ 2, 0 ≦ d <1 ). It is preferable to use a lithium-manganese composite oxide having a spinel structure .
[0013]
In mixing the lithium / nickel composite oxide and the lithium / manganese composite oxide, the weight ratio of the lithium / nickel composite oxide to the lithium / manganese composite oxide is 1: 9 to 9: 1. The range is preferably set to 6: 4.
[0014]
In addition, when mixing and sintering the lithium-nickel composite oxide and the lithium-manganese composite oxide in this way, if the firing temperature is low, the lithium-nickel composite oxide and the lithium-manganese composite oxide are sufficient. On the other hand, if the firing temperature becomes too high, oxygen in the lithium / nickel composite oxide or lithium / manganese composite oxide is desorbed and deteriorates, so the firing temperature is 200 to 900 ° C., preferably 400 to 600. Sinter at ℃.
[0015]
【Example】
Hereinafter, the nonaqueous electrolyte secondary battery according to the present invention will be specifically described with reference to examples, and in the case of the nonaqueous electrolyte secondary battery in this example, the potential of the positive electrode rapidly decreases at the end of discharge. It will be clarified with a comparative example that this is suppressed. In addition, the nonaqueous electrolyte secondary battery in this invention is not limited to what was shown in the following Example, It can implement by changing suitably in the range which does not change the summary.
[0016]
Example 1
In Example 1, in preparing the positive electrode, LiNi 0.4 Co 0.3 Mn 0.3 O 2 and Li 1.1 Mn 1.9 O 4 were mixed in a weight ratio of 6: 4 and formed into a pellet. Firing was performed in an air atmosphere at 500 ° C. to obtain a sintered material in which LiNi 0.4 Co 0.3 Mn 0.3 O 2 and Li 1.1 Mn 1.9 O 4 were mixed and sintered.
[0017]
And this sintered material and the artificial graphite of a electrically conductive agent were mixed by the weight ratio of 9: 1, and the positive mix was obtained.
[0018]
Next, an N-methyl-2-pyrrolidone solution containing 5% by weight of polyvinylidene fluoride was added to the positive electrode mixture so that the positive electrode mixture and the polyvinylidene fluoride binder were in a weight ratio of 95: 5. In addition, this was kneaded to prepare a slurry. This slurry was applied to both surfaces of an aluminum foil having a thickness of 20 μm by a doctor blade method, and this was vacuum-dried at 150 ° C. for 2 hours to produce a positive electrode.
[0019]
(Comparative Example 1)
In Comparative Example 1, when the positive electrode was produced, LiNi 0.4 Co 0.3 Mn 0.3 O 2 and Li 1.1 Mn 1.9 O 4 were mixed in a weight ratio of 6: 4 in the same manner as in Example 1 above. On the other hand, this was used without firing, and thereafter, a positive electrode was produced in the same manner as in Example 1 above.
[0020]
As shown in FIG. 1, each of the positive electrodes prepared in Example 1 and Comparative Example 1 is used as the working electrode 11, while metallic lithium is used for the counter electrode 12 and the reference electrode 13, which are negative electrodes, As the
[0021]
In each of the test batteries of Example 1 and Comparative Example 1 using each of the positive electrodes as the working electrode 11, the battery was charged at a charging current of 0.75 mA / cm 2 until the end-of-charge voltage was 4.3V. The battery was charged at a charging current of 0.25 mA / cm 2 until the end-of-charge voltage was 4.3V. Thereafter, the test batteries of Example 1 and Comparative Example 1 were discharged at a discharge current of 0.75 mA / cm 2 until the discharge end voltage reached 3.1 V, and the potential of each positive electrode 11 with respect to the reference electrode 13 during discharge was The relationship with the depth of discharge (%) was examined, and the result of the test battery of Example 1 is shown by a solid line, and the result of the test battery of Comparative Example 1 is shown by a broken line in FIG.
[0022]
As a result, in the test battery of Example 1, the decrease in the potential of the positive electrode when the discharge depth approached 100% was more gradual than that of the test battery of Comparative Example 1. In the case of the test battery, compared to the test battery of Comparative Example 1, overdischarge could be easily suppressed.
[0023]
【The invention's effect】
As described above in detail, in the nonaqueous electrolyte secondary battery according to the present invention, a sintered material obtained by mixing and sintering a lithium / manganese composite oxide and a lithium / nickel composite oxide is used as the material of the positive electrode. As a result, the decrease in the potential of the positive electrode at the end of the discharge was moderate as compared with the case where a mixture of lithium / manganese composite oxide and lithium / nickel composite oxide was simply used.
[0024]
As a result, in the nonaqueous electrolyte secondary battery according to the present invention, even when the depth of discharge is increased, it is possible to easily control the capacity reduction due to overdischarge, and the nonaqueous electrolyte secondary battery having excellent charge / discharge cycle characteristics. Batteries can be obtained.
[Brief description of the drawings]
FIG. 1 is a schematic explanatory view of a test battery produced in Example 1 and Comparative Example 1 of the present invention.
FIG. 2 is a graph showing the relationship between the potential of the positive electrode and the depth of discharge (%) when the test batteries of Example 1 and Comparative Example 1 are discharged.
[Explanation of symbols]
11 Working electrode (positive electrode)
12 Counter electrode (negative electrode)
13
Claims (3)
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| JP2001336620A JP4049571B2 (en) | 2001-11-01 | 2001-11-01 | Nonaqueous electrolyte secondary battery |
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| JP2001336620A JP4049571B2 (en) | 2001-11-01 | 2001-11-01 | Nonaqueous electrolyte secondary battery |
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| JP2003142091A JP2003142091A (en) | 2003-05-16 |
| JP4049571B2 true JP4049571B2 (en) | 2008-02-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AU2003221171A1 (en) | 2002-03-27 | 2003-10-08 | Yuasa Corporation | Active substance of positive electrode and nonaqueous electrolyte battery containing the same |
| JP4249727B2 (en) * | 2005-05-13 | 2009-04-08 | 株式会社東芝 | Nonaqueous electrolyte battery and lithium titanium composite oxide |
| JP5315591B2 (en) * | 2006-02-20 | 2013-10-16 | ソニー株式会社 | Positive electrode active material and battery |
| WO2013137510A1 (en) * | 2012-03-13 | 2013-09-19 | 주식회사 엘앤에프신소재 | Method for manufacturing anode active material for lithium secondary battery, anode active material for lithium secondary battery, and lithium secondary battery |
| WO2013137509A1 (en) | 2012-03-13 | 2013-09-19 | 주식회사 엘앤에프신소재 | Method for manufacturing anode active material for lithium secondary battery, anode active material for lithium secondary battery, and lithium secondary battery |
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