JP2000215891A - Manufacture of lithium secondary battery positive electrode material - Google Patents
Manufacture of lithium secondary battery positive electrode materialInfo
- Publication number
- JP2000215891A JP2000215891A JP11016525A JP1652599A JP2000215891A JP 2000215891 A JP2000215891 A JP 2000215891A JP 11016525 A JP11016525 A JP 11016525A JP 1652599 A JP1652599 A JP 1652599A JP 2000215891 A JP2000215891 A JP 2000215891A
- Authority
- JP
- Japan
- Prior art keywords
- compound
- secondary battery
- positive electrode
- electrode material
- compounds
- 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.)
- Withdrawn
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Classifications
-
- 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、リチウム二次電池
で代表される非水電解液二次電池に用いられるＬｉ二次
電池正極材料に関する。The present invention relates to a positive electrode material for a Li secondary battery used for a non-aqueous electrolyte secondary battery represented by a lithium secondary battery.
【０００２】[0002]
【従来の技術】近年、ＡＶ機器或いはパソコン等の電子
機器のポータブル化、コードレス化が急速に進んでお
り、これらの駆動用電源として小型、軽量で高エネルギ
ー密度を有する二次電池への要求が高い。このような要
求に対して、非水系二次電池、特にリチウム二次電池
（以下「Ｌｉ二次電池」という）は、とりわけ高電圧，
高エネルギー密度を有する電池としての期待が大きい。
これらの要求を満足するリチウム二次電池用の正極材料
としてリチウムをインターカレーション，デインターカ
レーションすることのできるＬｉＣｏＯ2 ，ＬｉＮｉＯ
2 或いはこれらの酸化物に遷移金属元素を一部置換した
複合酸化物等の層状化合物の研究が盛んに行われてい
る。2. Description of the Related Art In recent years, portable and cordless electronic devices such as AV devices and personal computers have been rapidly advanced, and there has been a demand for small, lightweight, high energy density secondary batteries as power sources for driving these devices. high. In response to such demands, non-aqueous secondary batteries, particularly lithium secondary batteries (hereinafter referred to as “Li secondary batteries”), have high voltage,
Expectations are high for batteries with high energy density.
LiCoO 2 and LiNiO capable of intercalating and de-intercalating lithium as a positive electrode material for a lithium secondary battery satisfying these requirements.
2. Description of the Related Art Layered compounds such as composite oxides in which a transition metal element is partially substituted for these oxides or these oxides have been actively studied.
【０００３】また、層状構造を持たないが、ＬｉＣｏＯ
2 等と同様な４Ｖ級の高電圧を有する安価な材料とし
て、Ｌｉ−Ｍｎ複合酸化物であるＬｉＭｎ2 Ｏ4 や、ま
た電圧は約３Ｖと若干低いＬｉＭｎＯ2 の開発も進めら
れている。[0003] Further, although having no layered structure, LiCoO
As an inexpensive material having a high voltage of 4V class similar to 2 or the like, development of LiMn 2 O 4 which is a Li—Mn composite oxide and LiMnO 2 having a slightly lower voltage of about 3 V are also in progress.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、これら
Ｌｉ−Ｍｎ複合酸化物をリチウム二次電池用の正極材料
として用いた場合において、従来のＬｉＣｏＯ2 ，Ｌｉ
ＮｉＯ2 を正極材料として用いた場合と比較して高温電
池特性に劣るという問題があった。この対策として、Ｍ
ｎの一部をＬｉで置換したり、遷移元素で置換するとい
う方法も試みれらたが、ある程度の改善は得られるもの
の未だ充分ではない。また、電池容量も小さいという問
題がある。However, when these Li-Mn composite oxides are used as a cathode material for a lithium secondary battery, conventional LiCoO 2 , Li
There is a problem that the high-temperature battery characteristics are inferior to the case where NiO 2 is used as the cathode material. As a measure against this, M
Attempts have been made to replace part of n with Li or with a transition element, but some improvements have been obtained but are still not sufficient. There is also a problem that the battery capacity is small.
【０００５】[0005]
【課題を解決するための手段】上記課題を解決する［請
求項１］のＬｉ二次電池正極材料の製造方法の発明は、
Ｍｎ化合物とＬｉ化合物とに、Ｎａ，Ｋ化合物の少なく
とも一種と、Ａｌ，Ｃｏ，Ｃｒ，Ｎｉ，Ｆｅ，Ｍｇ化合
物の少なくとも一種とを加えて混合し、該混合物を８５
０℃〜１１００℃の範囲で焼成を行うことを特徴とす
る。Means for Solving the Problems The invention of a method for producing a positive electrode material for a Li secondary battery according to claim 1 which solves the above-mentioned problems,
At least one of Na and K compounds and at least one of Al, Co, Cr, Ni, Fe and Mg compounds are added to and mixed with the Mn compound and the Li compound.
The sintering is performed in a range of 0 ° C. to 1100 ° C.
【０００６】［請求項２］のＬｉ二次電池正極材料の発
明は、請求項１の方法により製造してなることを特徴と
する。A second aspect of the invention for a positive electrode material for a Li secondary battery is characterized by being manufactured by the method of the first aspect.
【０００７】［請求項３］のＬｉ二次電池の発明は、請
求項２のＬｉ二次電池正極材料を用いてなることを特徴
とする。According to a third aspect of the present invention, there is provided a Li secondary battery comprising the Li secondary battery positive electrode material according to the second aspect.
【０００８】[0008]
【発明の実施の形態】以下、本発明の実施の形態を説明
する。Embodiments of the present invention will be described below.
【０００９】本発明のＬｉ二次電池正極材料の製造方法
の発明は、Ｍｎ化合物とＬｉ化合物とに、Ｎａ，Ｋ化合
物の少なくとも一種と、Ａｌ，Ｃｏ，Ｃｒ，Ｎｉ，Ｆ
ｅ，Ｍｇ化合物の少なくとも一種とを加えて混合し、該
混合物を８５０℃〜１１００℃の範囲で焼成を行うもの
である。すなわち、Ｍｎ化合物とＬｉ化合物とを主成分
とし、さらに、Ｎａ，Ｋ化合物の少なくとも一種を第１
添加成分とし、Ａｌ，Ｃｏ，Ｃｒ，Ｎｉ，Ｆｅ，Ｍｇ化
合物の少なくとも一種を第２添加成分とした混合物を８
５０℃〜１１００℃の範囲で焼成することにより、Ｌｉ
二次電池正極材料を提供するものである。ここで、上記
Ｎａ化合物等の第１添加成分の添加量としては、放電容
量及び容量維持率との関係から0.０５〜２重量％とする
のが好ましい。ここで、上記Ａｌ化合物等の第２添加成
分の添加量としては、放電容量及び容量維持率との関係
から0.０５〜６重量％とするのが好ましい。The invention of the method for producing a cathode material for a Li secondary battery according to the present invention is characterized in that a Mn compound and a Li compound, at least one of Na and K compounds, and Al, Co, Cr, Ni, F
e and at least one of the Mg compounds are added and mixed, and the mixture is fired at a temperature in the range of 850 ° C to 1100 ° C. That is, a main component is a Mn compound and a Li compound, and at least one of Na and K compounds is a first compound.
A mixture containing at least one of Al, Co, Cr, Ni, Fe, and Mg compounds as a second additive component as an additive component was added to the mixture.
By firing in the range of 50 ° C. to 1100 ° C., Li
It is intended to provide a secondary battery positive electrode material. Here, the addition amount of the first addition component such as the above Na compound is preferably 0.05 to 2% by weight in view of the relationship between the discharge capacity and the capacity retention rate. Here, the addition amount of the second addition component such as the Al compound is preferably 0.05 to 6% by weight in view of the relationship between the discharge capacity and the capacity retention rate.
【００１０】ここで、第１段階の焼成温度の範囲を８５
０℃〜１１００℃とするのは、後述する実施例に示すよ
うに、８５０℃未満であると、Ｍｎ化合物とＬｉ化合物
と第１添加成分及び第２添加成分の反応が充分でなく、
６０℃での容量維持率が低いからであり、一方、１１０
０℃を超えて焼成すると、Ｌｉの昇華が起こり、２０℃
及び６０℃での電池特性が悪くなり、共に好ましくない
からである。[0010] Here, the range of the firing temperature in the first stage is 85
When the temperature is set to 0 ° C. to 1100 ° C., as shown in Examples described below, if the temperature is lower than 850 ° C., the reaction between the Mn compound, the Li compound, the first additive component and the second additive component is not sufficient,
This is because the capacity retention at 60 ° C. is low.
When calcined above 0 ° C., sublimation of Li occurs, and
And the battery characteristics at 60 ° C. are deteriorated, which are both undesirable.
【００１１】また、非水電解液二次電池であるＬｉ二次
電池の発明は、上記Ｌｉ二次電池用正極材料を正極活物
質として用いてなるものである。なお、本発明における
Ｌｉ二次電池の負極には、金属リチウム又はリチウムを
吸蔵放出可能な物質を用いれば何等限定されるものでは
なく、電解質についても、例えばカーボネート類，スル
ホラン類，ラクトン類，エーテル類の有機溶媒中にリチ
ウム塩を溶解したものや、リチウムイオン導電性の固体
電解質を用いることができ、本発明において何等制限さ
れるものではない。Further, the invention of a Li secondary battery which is a non-aqueous electrolyte secondary battery uses the above-mentioned positive electrode material for a Li secondary battery as a positive electrode active material. The negative electrode of the Li secondary battery according to the present invention is not particularly limited as long as metallic lithium or a substance capable of inserting and extracting lithium is used. For the electrolyte, for example, carbonates, sulfolane, lactone, ether A solution in which a lithium salt is dissolved in a kind of organic solvent or a solid electrolyte having lithium ion conductivity can be used, and is not limited in the present invention.
【００１２】[0012]
【実施例】以下、本発明の効果を示す実施例を説明する
が、本発明はこれに限定されるものではない。EXAMPLES Examples showing the effects of the present invention will be described below, but the present invention is not limited to these examples.
【００１３】（実施例１）Ｌｉ：Ｎａ：Ａｌ：Ｍｎ＝1.
００：0.０３：0.０５：1.９２となるように二酸化マン
ガン（９6.０ｇ）と炭酸リチウム（２1.２ｇ）と炭酸ナ
トリウム（1.４ｇ）と水酸化アルミニウム（2.１ｇ）を
秤量し、ボールミルで混合後、電気炉中で９００℃で焼
成し、解砕してＬｉ−Ｎａ−Ａｌ−Ｍｎ複合酸化物を生
成した。この得られた複合水酸化物を正極活物質として
コイン電池を作成し、放電試験を行った。試験内容とし
ては、２０℃における初期放電容量（ｍＡｈ／ｇ）及び
２０℃における１５サイクル時での容量維持率（％）、
並びに６０℃における１５サイクル時での容量維持率
（％）及び６０℃における３日間充電保存時の容量回復
率（％）を測定した。(Example 1) Li: Na: Al: Mn = 1.
Manganese dioxide (96.0 g), lithium carbonate (21.2 g), sodium carbonate (1.4 g), and aluminum hydroxide (2.1 g) were added so that the ratio became 00: 0.03: 0.05: 1.92. After weighing and mixing in a ball mill, the mixture was baked at 900 ° C. in an electric furnace and crushed to produce a Li—Na—Al—Mn composite oxide. A coin battery was prepared using the obtained composite hydroxide as a positive electrode active material, and a discharge test was performed. The test contents include an initial discharge capacity (mAh / g) at 20 ° C. and a capacity retention rate (%) at 15 cycles at 20 ° C.
The capacity retention rate (%) after 15 cycles at 60 ° C. and the capacity recovery rate (%) after 3 days of charge storage at 60 ° C. were measured.
【００１４】（実施例２）焼成温度を８５０℃とした以
外は、実施例１と同様に操作した。Example 2 The operation was performed in the same manner as in Example 1 except that the firing temperature was 850 ° C.
【００１５】（実施例３）焼成温度を１１００℃とした
以外は、実施例１と同様に操作した。Example 3 The same operation as in Example 1 was carried out except that the firing temperature was 1100 ° C.
【００１６】（実施例４）炭酸ナトリウム（1.４ｇ）を
炭酸カリウム（1.９ｇ）とした以外は、実施例１と同様
に操作した。Example 4 The same operation as in Example 1 was carried out except that potassium carbonate (1.9 g) was used instead of sodium carbonate (1.4 g).
【００１７】（実施例５）水酸化アルミニウム（2.１
ｇ）を炭酸コバルト（3.３ｇ）とした以外は、実施例１
と同様に操作した。Example 5 Aluminum hydroxide (2.1)
g) was changed to cobalt carbonate (3.3 g).
The same operation was performed.
【００１８】（実施例６）水酸化アルミニウム（2.１
ｇ）を酸化クロム（2.２ｇ）とした以外は、実施例１と
同様に操作した。Example 6 Aluminum hydroxide (2.1)
The same operation as in Example 1 was carried out except that g) was changed to chromium oxide (2.2 g).
【００１９】（実施例７）水酸化アルミニウム（2.１
ｇ）を水酸化ニッケル（2.５ｇ）とした以外は、実施例
１と同様に操作した。Example 7 Aluminum hydroxide (2.1)
The same operation as in Example 1 was carried out except that g) was changed to nickel hydroxide (2.5 g).
【００２０】（実施例８）水酸化アルミニウム（2.１
ｇ）を酸化第一鉄（2.２ｇ）とした以外は、実施例１と
同様に操作した。Example 8 Aluminum hydroxide (2.1)
The same operation as in Example 1 was performed except that g) was changed to ferrous oxide (2.2 g).
【００２１】（実施例９）水酸化アルミニウム（2.１
ｇ）を酸化マグネシウム（1.１ｇ）とした以外は、実施
例１と同様に操作した。Example 9 Aluminum hydroxide (2.1)
The same operation as in Example 1 was carried out except that g) was changed to magnesium oxide (1.1 g).
【００２２】（比較例１）第１回目の焼成を８００℃と
した以外は、実施例１と同様に操作した。Comparative Example 1 The same operation as in Example 1 was performed except that the first baking was performed at 800 ° C.
【００２３】（比較例２）第１回目の焼成を１２００℃
とした以外は、実施例１と同様に操作した。(Comparative Example 2) The first baking was performed at 1200 ° C.
The same operation as in Example 1 was performed, except that
【００２４】（比較例３）Ｌｉ：Ｎａ：Ｍｎ＝1.００：
0.０３：1.９７となるように二酸化マンガン（９8.５
ｇ）と炭酸リチウム（２1.２ｇ）と炭酸ナトリウム（1.
４ｇ）を秤量し、ボールミルで混合後、電気炉中で９０
０℃で焼成し、解砕してＬｉ−Ｎａ−Ｍｎ複合酸化物を
生成した。試験方法は、実施例１と同様に行った。Comparative Example 3 Li: Na: Mn = 1.00:
Manganese dioxide (98.5) to give 0.03: 1.97.
g), lithium carbonate (21.2 g) and sodium carbonate (1.
4g) was weighed and mixed in a ball mill, and then mixed in an electric furnace.
It was baked at 0 ° C. and crushed to produce a Li—Na—Mn composite oxide. The test method was the same as in Example 1.
【００２５】（比較例４）Ｌｉ：Ａｌ：Ｍｎ＝1.００：
0.０５：1.９５となるように二酸化マンガン（９7.５
ｇ）と炭酸リチウム（２1.２ｇ）と水酸化アルミニウム
（2.１ｇ）を秤量し、ボールミルで混合後、電気炉中で
９００℃で焼成し、解砕してＬｉ−Ｍｎ−Ａｌ複合酸化
物を生成した。試験方法は、実施例１と同様に行った。Comparative Example 4 Li: Al: Mn = 1.00:
Manganese dioxide (97.5) to give 0.05: 1.95.
g), lithium carbonate (21.2 g), and aluminum hydroxide (2.1 g) were weighed, mixed in a ball mill, calcined in an electric furnace at 900 ° C., and crushed to obtain a Li—Mn—Al composite oxide. Generated. The test method was the same as in Example 1.
【００２６】以上実施例１乃至実施例９の結果並びに比
較例１乃至比較例４の結果を、下記「表１」に各々示
す。The results of Examples 1 to 9 and the results of Comparative Examples 1 to 4 are shown in Table 1 below.
【００２７】[0027]
【表１】 [Table 1]
【００２８】上記表より、本実施例にかかるものは、２
０℃での放電容量及び容量維持率、６０℃での容量維持
率及び充電保存後の容量回復率が共に好ましく、駆動用
電源としての好ましい二次電池特性を有することが、確
認できた。From the above table, according to the present embodiment, 2
It was confirmed that the discharge capacity and the capacity retention rate at 0 ° C., the capacity retention rate at 60 ° C., and the capacity recovery rate after charge storage were all favorable, and that the battery had favorable secondary battery characteristics as a power supply for driving.
【００２９】[0029]
【発明の効果】以上のように、本発明によれば、得られ
たＬｉ二次電池正極材料を正極活物質として使用するこ
とにより、高容量で且つ高温特性が良好であり、駆動用
電源として好ましい二次電池特性を提供することができ
る。As described above, according to the present invention, by using the obtained lithium secondary battery positive electrode material as a positive electrode active material, a high capacity and good high-temperature characteristics are obtained, and as a driving power source, Preferred secondary battery characteristics can be provided.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 5H003 AA00 AA02 BA01 BA03 BB05 BD01 5H014 AA01 BB01 BB06 EE10 HH08 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 5H003 AA00 AA02 BA01 BA03 BB05 BD01 5H014 AA01 BB01 BB06 EE10 HH08
Claims (3)
化合物の少なくとも一種と、Ａｌ，Ｃｏ，Ｃｒ，Ｎｉ，
Ｆｅ，Ｍｇ化合物の少なくとも一種とを加えて混合し、
該混合物を８５０℃〜１１００℃の範囲で焼成を行うこ
とを特徴とするＬｉ二次電池正極材料の製造方法。1. An Mn compound and a Li compound each containing Na, K
At least one compound, Al, Co, Cr, Ni,
At least one of Fe and Mg compounds is added and mixed,
A method for producing a positive electrode material for a Li secondary battery, comprising firing the mixture at a temperature in the range of 850C to 1100C.
を特徴とするＬｉ二次電池正極材料。2. A positive electrode material for a Li secondary battery, manufactured by the method according to claim 1.
てなることを特徴とするＬｉ二次電池。3. A Li secondary battery comprising the Li secondary battery positive electrode material according to claim 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11016525A JP2000215891A (en) | 1999-01-26 | 1999-01-26 | Manufacture of lithium secondary battery positive electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11016525A JP2000215891A (en) | 1999-01-26 | 1999-01-26 | Manufacture of lithium secondary battery positive electrode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000215891A true JP2000215891A (en) | 2000-08-04 |
Family
ID=11918703
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11016525A Withdrawn JP2000215891A (en) | 1999-01-26 | 1999-01-26 | Manufacture of lithium secondary battery positive electrode material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000215891A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004265863A (en) * | 2003-02-12 | 2004-09-24 | Matsushita Electric Ind Co Ltd | Lithium-ion secondary battery |
| JP2015530966A (en) * | 2013-07-26 | 2015-10-29 | エルジー・ケム・リミテッド | Polycrystalline lithium manganese oxide particles, method for producing the same, and positive electrode active material including the same |
| US9905850B2 (en) | 2013-07-26 | 2018-02-27 | Lg Chem, Ltd. | Polycrystalline lithium manganese oxide particles, preparation method thereof, and cathode active material including the same |
| US9905851B2 (en) | 2013-07-26 | 2018-02-27 | Lg Chem, Ltd. | Cathode active material and method of preparing the same |
-
1999
- 1999-01-26 JP JP11016525A patent/JP2000215891A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004265863A (en) * | 2003-02-12 | 2004-09-24 | Matsushita Electric Ind Co Ltd | Lithium-ion secondary battery |
| JP4549689B2 (en) * | 2003-02-12 | 2010-09-22 | パナソニック株式会社 | Lithium ion secondary battery |
| JP2015530966A (en) * | 2013-07-26 | 2015-10-29 | エルジー・ケム・リミテッド | Polycrystalline lithium manganese oxide particles, method for producing the same, and positive electrode active material including the same |
| US9905840B2 (en) | 2013-07-26 | 2018-02-27 | Lg Chem, Ltd. | Cathode active material and method of preparing the same |
| US9905850B2 (en) | 2013-07-26 | 2018-02-27 | Lg Chem, Ltd. | Polycrystalline lithium manganese oxide particles, preparation method thereof, and cathode active material including the same |
| US9905851B2 (en) | 2013-07-26 | 2018-02-27 | Lg Chem, Ltd. | Cathode active material and method of preparing the same |
| US10236499B2 (en) | 2013-07-26 | 2019-03-19 | Lg Chem, Ltd. | Polycrystalline lithium manganese oxide particles, preparation method thereof, and cathode active material including the same |
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