JP3943081B2 - Solid phase heating production method of lithium cobaltate - Google Patents
Solid phase heating production method of lithium cobaltate Download PDFInfo
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- JP3943081B2 JP3943081B2 JP2003578284A JP2003578284A JP3943081B2 JP 3943081 B2 JP3943081 B2 JP 3943081B2 JP 2003578284 A JP2003578284 A JP 2003578284A JP 2003578284 A JP2003578284 A JP 2003578284A JP 3943081 B2 JP3943081 B2 JP 3943081B2
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Description
【０００１】
【産業上の利用分野】
本発明は、非水状態におけるカソード材料、ロッキングチェア型二次電池またはインターカレーション型二次電池(secondary rock in chair or intercalated batteries)のための固相及びポリマー電解質として有用な、コバルト酸リチウム（ＬｉＣｏＯ2 ）の製造のための新しい固相熱方法に関する。
【０００２】
【従来の技術】
コバルト酸リチウム（ＬｉＣｏＯ2）は、リチウムイオンに対するその高い可逆性と、ＬｉＮｉＯ2及びＬｉＭｎ２Ｏ4電極よりも放電容量の低減が少ないという観点から、リチウム二次電池の正極として広く用いられている。コバルト酸リチウム（ＬｉＣｏＯ2）のカソードを製造するための技術分野において報告されている方法は、長い継続時間で３５０〜５００℃の温度範囲でのゾル‐ゲル法などの穏やかな化学反応による、硝酸リチウム、水酸化リチウム、酢酸リチウムまたは他のリチウム塩と、コバルトの硝酸塩、酸化塩、酢酸塩、水酸化塩、硫酸塩との反応及び、多段階の製造方法を開示する。通常、これら酸化物の合成における固相での熱的方法で、反応は、長時間の加熱、断続的な冷却及び粉砕処理により継続される。パルスレーザー蒸着、スパッタリング及び、静電スプレー蒸着などのコバルト酸リチウムの合成のために、他の製造方法がまた文献で入手できる。
【０００３】
〔参考文献〕
1."Synthesis and electrochemical properties of LiCoO2 spinel cathodes"S. Chol and A. Manthiram, Journal of the Electrochemical Society, Vol.149(2) (2002) A162−166
2."X-ray absorption spectroscopic study of LiAlyCo1-yO2cathode for lithium rechargeable batteries"Won-Sub Yoon, Kyung-Keun Lee and Kwang-Bum Kim, Journal of the Electrochemical Society,Vol. 149(2)(2002)A146-151
3."High temperature combustion synthesis and electrochemical characterization of LiNiO2, LiCoO2 and LiMn2O4for lithium ion secondary batteries"M.M.Rao, C. Liebenow, M. Jayalakshimi, M. Wulff, U. Guth and F. Scholz,J. of Solid State Electrochemistry, Vol. 5, Issue 5(2001) 348-354
4."Fabrication of LiCoO2 thin films by solgel method and characterization as positive electrodes for Li/LiCoO2cells"M.N. Kim,H.Chung, Y. Park, J.Kim, J. Son, K. Park and H. Kim, Journal of Power Sources, Vol. 99(2001)34-40
5."Preparation and characterization of high density spherical LiNi0.8CoO2cathode material for lithium secondary batteries"Jierong Ying, Chunrong Wan, Changyin Jiang and Yangxing Li,J. of Power Sources, Vol. 99(2001)78-84
6."Electrochemical characterization of layered LiCoO2 films prepared by electrostatic deposition"Won-Sub Yoon, Sung-Ho Ban, Kyung-Keun Lee, Kwang-Bum Kim, Min-Dyu Kim and Jay Min Lee, J. of Power Sources, Vol. 97-98(2001)282-286
7."Emulsion-derived lithium manganese oxide powder for positive electrodes in lithium ion batteries"Chung-Hsin Lu and Shang-Wei Lin, J. of Power Sources, Vol. 93(2001)14-19
8."Cobalt doped chromium oxides as cathode materials for secondsry batteries for secondary lithium batteries",Dong Zhang, Branko N. Popov, Yury M. Poddrahnsky, Pankaj Arora and Ralph E. White,. J. of Power Sources, Vol. 83(1999)121-127
9."Synthesis and electrochemical studies of spinel phase LiMn2O4cathodematerials prepared by the pechini process". W. Liu, G.C. Farringon, F.Chaput and B. Dunn, Journal of the Electrochemical Society, Vol. 143, No.3(1996)879-884
【０００４】
上記で報告された従来の方法には幾つかの不都合がある。一般的に、つぎのいずれか１つまたは全てが見られる。
【０００５】
１．例えば予期しない組成及び望まれない副生成物等の副反応が生じる。
２．未反応物質が残り、不純物として作用する。
３．不完全な反応を生ずる。
４．幾つかの段階と長い焼成時間とが、製造のために必要とされる。
５．制御された条件が必要とされる。
６．望まれない相が形成される。
【０００６】
そのため、上に列挙した不都合を克服する方法の開発が重要である。
【０００７】
【発明が解決しようとする課題】
本発明の主たる目的は、上述した欠陥を回避する、従来試みられなかったコバルト酸リチウム（ＬｉＣｏＯ2）の製造のための新しい方法を提供するにある。
【０００８】
本発明の他の目的は、多段階での処理、望まれず予期しない副生成物及び先行技術に報告される望まれない相の形成を回避することである。
【０００９】
【課題を解決するための手段】
上記及びその他の本発明の目的は、酸化リチウムと硝酸コバルトとの１段階の固相熱反応からなる本発明の新しい方法により達成される。
【００１０】
従って、本発明は、酸化リチウム（ＬｉＯ2）と硝酸コバルト（Ｃｏ（ＮＯ3）2）とを固相で均一に混合し、該混合物に熱発生物質を添加して粉砕し、粉砕した前記混合物を６５０〜７００℃の範囲の温度に加熱してコバルト酸リチウムを得ることからなる１段階の固相熱反応によるコバルト酸リチウムの製造方法に関する。
【００１１】
本発明の一実施形態において、酸化リチウム及び硝酸コバルトの混合物と、熱発生物質との比率は１：３である。
本発明の他の実施形態において、粉砕した混合物を炉中で約８時間加熱する。
本発明の一実施形態において、酸化リチウムは下記の比率で硝酸コバルトと混合される。
【００１２】
ＬｉＯ2：Ｃｏ（ＮＯ3）2 ＝１：２
【００１３】
本発明の他の実施形態において、熱発生物質は尿素または硝酸アンモニウムから選択される。
本発明の更なる他の実施形態において、電気炉が加熱のために使用される。
本発明の更なる他の実施形態において、用いられる原料は全て固体である。
【００１４】
【発明の実施の形態】
本発明は、酸化リチウム（ＬｉＯ2）と硝酸コバルト（Ｃｏ（ＮＯ3）2）とを固相で均一に混合し、該混合物に尿素または硝酸アンモニウムのような熱発生物質を添加して粉砕し、粉砕した前記混合物を６５０〜７００℃の範囲の温度に加熱して、所望のコバルト酸リチウムを得ることからなるコバルト酸リチウムの製造のための１段階の固相熱反応を含む。ＬＩ2Ｏ＋Ｃｏ（ＮＯ3）2混合物と尿素の比率は好ましくは１：３である。粉砕した混合物は炉中で約８時間加熱される。Ｌｉ2Ｏは下記の好ましい比率でＣｏ（ＮＯ3）2と混合される。
【００１５】
ＬｉＯ2：Ｃｏ（ＮＯ3）2 ＝１：２
【００１６】
加熱は、固相である用いられるすべての原料と共に、好ましくは電気炉中で行われる。は固体で使用される。
熱反応の間に下記反応が起きる。
【００１７】
ＬｉＯ2＋２Ｃｏ（ＮＯ3）2＋３（Ｏ） → ２ＬｉＣｏＯ2＋４ＮＯ2＋２Ｏ2
この反応は単一段階で進行するものと見られ、生成物はＸ線回折によりコバルト酸リチウムと確認された。
【００１８】
固相材料のＬｉＯ2 は、制御された条件下、穏やかな温度で、固体のＣｏ（ＮＯ3 ）2 と反応せしめられ、非常に優れたインターカレーション型の正極として有用なまさしく非常に優れたスピネル構造のサンプルを得る。純粋な分析試薬のＣｏ（ＮＯ3 ）2のサンプルを、純粋な分析試薬のＬｉＯ2 のサンプルと、２：１のモル比で混合し、重量パーセントで３倍の尿素と均一な混合物を形成する。より良い均質な混合物を得るために、この混合物を２回蒸留した無水ジエチレンカーボネート（ＤＥＣ）と共に十分に粉砕する。この混合物を３００℃に加熱し、更に７００℃で５時間連続的に加熱して、Ｘ線解析（図１ａ）により証明されるコバルト酸リチウム（ＬｉＣｏＯ2 ）を得る。
【００１９】
この反応は、尿素を硝酸アンモニウムに代えても行うことができる。固相材料のＬｉＯ2 は、制御された条件下、穏やかな温度で、固体のＣｏ（ＮＯ3 ）2 と反応せしめられ、非常に優れたインターカレーション型の正極として有用なまさしく非常に優れたスピネル構造のサンプルを得る。純粋な分析試薬のＣｏ（ＮＯ3 ）2のサンプルを、純粋な分析試薬のＬｉＯ2のサンプルと、２：１のモル比で混合し、重量パーセントで３倍の硝酸アンモニウムと均一な混合物を形成する。より良い均質な混合物を得るために、この混合物を２回蒸留した無水ジエチレンカーボネート（ＤＥＣ）と共に十分に粉砕する。この混合物を３００℃に加熱し、更に７００℃で５時間連続的に加熱して、Ｘ線解析（図１ｂ）により証明されるコバルト酸リチウム（ＬｉＣｏＯ2 ）を得る。
【００２０】
以下の実施例は本発明を説明するためのものであり、本発明の技術的範囲を限定するものと解釈されるべきではない。
【００２１】
実施例１：ＬｉＣｏＯ2の製造
【００２２】
固相材料のＬｉＯ2 は、制御された条件下、穏やかな温度で、固体のＣｏ（ＮＯ3 ）2 と反応せしめられ、非常に優れたインターカレーション型の正極として有用なまさしく非常に優れたスピネル構造のサンプルを得る。純粋な分析試薬のＣｏ（ＮＯ3 ）2のサンプルを、純粋な分析試薬のＬｉＯ2 のサンプルと、２：１のモル比で混合し、重量パーセントで３倍の尿素と均一な混合物を形成する。より良い均質な混合物を得るために、この混合物を２回蒸留した無水ジエチレンカーボネート（ＤＥＣ）と共に十分に粉砕する。この混合物を３００℃で３時間加熱し、次に７００℃で５時間連続的に加熱して、コバルト酸リチウム（ＬｉＣｏＯ2 ）を得た。コバルト酸リチウムは、Ｘ線解析（図１ａ）により証明される。
【００２３】
実施例２：ＬｉＣｏＯ2の製造
【００２４】
固相材料のＬｉＯ2 は、制御された条件下、穏やかな温度で、固体のＣｏ（ＮＯ3 ）2 と反応せしめられ、非常に優れたインターカレーション型の正極として有用なまさしく非常に優れたスピネル構造のサンプルを得る。純粋な分析試薬のＣｏ（ＮＯ3 ）2のサンプルを、純粋な分析試薬のＬｉＯ2のサンプルと、２：１のモル比で混合し、重量パーセントで３倍の硝酸アンモニウムと均一な混合物を形成する。より良い均質な混合物を得るために、この混合物を２回蒸留した無水ジエチレンカーボネート（ＤＥＣ）と共に十分に粉砕する。この混合物を３００℃に加熱し、次に７００℃で５時間連続的に加熱して、コバルト酸リチウム（ＬｉＣｏＯ2 ）を得た。コバルト酸リチウムは、Ｘ線解析（図１ｂ）により証明される。
【００２５】
実施例３
【００２６】
純粋で乾燥された分析試薬のＬｉＯ2 を、純粋で乾燥された分析試薬のＣｏ（ＮＯ3 ）2と、乳鉢と乳棒とを用いて１：２のモル比で混合し、ついで、混合物に、さらに重量で３倍の尿素を混合し、電気炉内に入れた。この混合物を最初に３００℃で３時間加熱し、続いて７００℃で５時間加熱した。
【００２７】
【表１】
実施例４
【００２９】
純粋で乾燥された分析試薬のＬｉＯ2 を、純粋で乾燥された分析試薬のＣｏ（ＮＯ3 ）2と、乳鉢と乳棒とを用いて１：２のモル比で混合し、ついで、混合物に、さらに重量で３倍の硝酸アンモニウムを混合した。最終的な混合物を最初に３００℃で３時間加熱し、続いて７００℃で５時間加熱した。
【００３０】
【表２】
結論
【００３２】
１．酸化リチウムは、１：２の等モル比でＣｏ（ＮＯ3 ）2と反応し、ＬｉＣｏＯ2を形成する。
２．尿素、硝酸アンモニウム及び同様の熱発生物質は、効率または生成品の組成を大きく変えることなく、自己発熱物質として使用することができ、これらの物質はスピネル構造の形成に重要である。
３．形成温度は６５０℃乃至７００℃の範囲である。
４．加熱時間は約８時間のみである。
【００３３】
【発明の効果】
本発明の主たる効果は以下の通りである。
１．本発明の製造方法は単一段階の固相熱反応である。
２．ＬｉＯ2 は、インターカレーションのための高容量正極のＬｉＣｏＯ2を形成するために、Ｃｏ（ＮＯ3 ）2との反応に使用できる。
３．加熱時間は８時間のみで、この故に、かなりの加熱時間が節約できる。
【図面の簡単な説明】
【図１】 本発明にかかる方法によって得られたコバルト酸リチウムのＸ線回折パターンである。[0001]
[Industrial application fields]
The present invention relates to a lithium cobalt oxide (cathode material useful as a solid phase and polymer electrolyte for a non-aqueous cathode material, a rocking chair type secondary battery or an intercalated type secondary battery. It relates to a new solid phase thermal process for the production of LiCoO 2 ).
[0002]
[Prior art]
Lithium cobaltate (LiCoO 2 ) is widely used as the positive electrode of lithium secondary batteries from the viewpoint of its high reversibility to lithium ions and less reduction in discharge capacity than LiNiO 2 and LiMn 2 O 4 electrodes. . A method reported in the technical field for producing a lithium cobaltate (LiCoO 2 ) cathode is nitric acid by a mild chemical reaction such as a sol-gel process in the temperature range of 350-500 ° C. with a long duration. Reactions of lithium, lithium hydroxide, lithium acetate or other lithium salts with cobalt nitrates, oxides, acetates, hydroxides, sulfates and multi-step production processes are disclosed. Usually, the reaction is continued by heating for a long time, intermittent cooling and pulverization in a solid phase thermal method in the synthesis of these oxides. Other manufacturing methods are also available in the literature for the synthesis of lithium cobaltate, such as pulsed laser deposition, sputtering and electrostatic spray deposition.
[0003]
[References]
1. "Synthesis and electrochemical properties of LiCoO 2 spinel cathodes" S. Chol and A. Manthiram, Journal of the Electrochemical Society, Vol.149 (2) (2002) A162−166
2. "X-ray absorption spectroscopic study of LiAl y Co 1-y O 2 cathode for lithium rechargeable batteries" Won-Sub Yoon, Kyung-Keun Lee and Kwang-Bum Kim, Journal of the Electrochemical Society, Vol. 149 (2 (2002) A146-151
3. "High temperature combustion synthesis and electrochemical characterization of LiNiO 2, LiCoO 2 and LiMn 2 O 4 for lithium ion secondary batteries" MMRao, C. Liebenow, M. Jayalakshimi, M. Wulff, U. Guth and F. Scholz, J of Solid State Electrochemistry, Vol. 5, Issue 5 (2001) 348-354
4. "Fabrication of LiCoO 2 thin films by solgel method and characterization as positive electrodes for Li / LiCoO 2 cells" MN Kim, H. Chung, Y. Park, J. Kim, J. Son, K. Park and H. Kim , Journal of Power Sources, Vol. 99 (2001) 34-40
5. "Preparation and characterization of high density spherical LiNi 0.8 CoO 2 cathode material for lithium secondary batteries" Jierong Ying, Chunrong Wan, Changyin Jiang and Yangxing Li, J. of Power Sources, Vol. 99 (2001) 78-84
6. "Electrochemical characterization of layered LiCoO 2 films prepared by electrostatic deposition" Won-Sub Yoon, Sung-Ho Ban, Kyung-Keun Lee, Kwang-Bum Kim, Min-Dyu Kim and Jay Min Lee, J. of Power Sources, Vol. 97-98 (2001) 282-286
7. "Emulsion-derived lithium manganese oxide powder for positive electrodes in lithium ion batteries" Chung-Hsin Lu and Shang-Wei Lin, J. of Power Sources, Vol. 93 (2001) 14-19
8. "Cobalt doped chromium oxides as cathode materials for secondsry batteries for secondary lithium batteries", Dong Zhang, Branko N. Popov, Yury M. Poddrahnsky, Pankaj Arora and Ralph E. White ,. J. of Power Sources, Vol. 83 (1999) 121-127
9. "Synthesis and electrochemical studies of spinel phase LiMn 2 O 4 cathodematerials prepared by the pechini process". W. Liu, GC Farringon, F. Chaput and B. Dunn, Journal of the Electrochemical Society, Vol. 143, No. 3 (1996) 879-884
[0004]
There are several disadvantages to the conventional method reported above. In general, any one or all of the following are found:
[0005]
1. For example, side reactions such as unexpected compositions and unwanted side products occur.
2. Unreacted material remains and acts as an impurity.
3. Incomplete reaction occurs.
4). Several steps and long firing times are required for production.
5). Controlled conditions are required.
6). Undesirable phases are formed.
[0006]
Therefore, it is important to develop a method that overcomes the disadvantages listed above.
[0007]
[Problems to be solved by the invention]
The main object of the present invention is to provide a new method for the production of lithium cobaltate (LiCoO 2 ) which has not been tried before, avoiding the above-mentioned defects.
[0008]
Another object of the present invention is to avoid multi-stage processing, formation of unwanted and unexpected by-products and unwanted phases reported in the prior art.
[0009]
[Means for Solving the Problems]
These and other objects of the present invention are achieved by the new process of the present invention which comprises a one-step solid state thermal reaction of lithium oxide and cobalt nitrate.
[0010]
Accordingly, the present invention provides a mixture of lithium oxide (LiO 2 ) and cobalt nitrate (Co (NO 3 ) 2 ) that are uniformly mixed in a solid phase, pulverized by adding a heat generating material to the mixture, and pulverized The present invention relates to a method for producing lithium cobaltate by a one-step solid-phase thermal reaction comprising heating lithium to a temperature in the range of 650 to 700 ° C. to obtain lithium cobaltate.
[0011]
In one embodiment of the present invention, the ratio of the mixture of lithium oxide and cobalt nitrate to the heat generating material is 1: 3.
In another embodiment of the invention, the ground mixture is heated in an oven for about 8 hours.
In one embodiment of the present invention, lithium oxide is mixed with cobalt nitrate in the following ratios.
[0012]
LiO 2 : Co (NO 3 ) 2 = 1: 2
[0013]
In another embodiment of the invention, the heat generating material is selected from urea or ammonium nitrate.
In yet another embodiment of the invention, an electric furnace is used for heating.
In yet another embodiment of the invention, the raw materials used are all solid.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
In the present invention, lithium oxide (LiO 2 ) and cobalt nitrate (Co (NO 3 ) 2 ) are uniformly mixed in a solid phase, and a heat-generating substance such as urea or ammonium nitrate is added to the mixture and pulverized. Heating the pulverized mixture to a temperature in the range of 650-700 ° C. to include a one-step solid state thermal reaction for the production of lithium cobaltate comprising obtaining the desired lithium cobaltate. The ratio of LI 2 O + Co (NO 3 ) 2 mixture to urea is preferably 1: 3. The ground mixture is heated in an oven for about 8 hours. Li 2 O is mixed with the Co (NO 3) 2 in a preferred ratio of below.
[0015]
LiO 2 : Co (NO 3 ) 2 = 1: 2
[0016]
Heating is preferably performed in an electric furnace with all raw materials used in solid phase. Is used in solids.
The following reactions occur during the thermal reaction:
[0017]
LiO 2 + 2Co (NO 3 ) 2 +3 (O) → 2LiCoO 2 + 4NO 2 + 2O 2
This reaction appeared to proceed in a single step, and the product was confirmed to be lithium cobaltate by X-ray diffraction.
[0018]
The solid-state material LiO 2 is reacted with solid Co (NO 3 ) 2 under controlled conditions at moderate temperatures and is very excellent as a very good intercalation type positive electrode A sample with a spinel structure is obtained. A sample of pure analytical reagent Co (NO 3 ) 2 is mixed with a sample of pure analytical reagent LiO 2 in a 2: 1 molar ratio to form a homogeneous mixture with 3 times weight percent of urea. . In order to obtain a better homogeneous mixture, this mixture is thoroughly ground with double distilled anhydrous diethylene carbonate (DEC). The mixture is heated to 300 ° C. and then continuously heated at 700 ° C. for 5 hours to obtain lithium cobaltate (LiCoO 2 ) as evidenced by X-ray analysis (FIG. 1a).
[0019]
This reaction can also be performed by replacing urea with ammonium nitrate. The solid-state material LiO 2 is reacted with solid Co (NO 3 ) 2 under controlled conditions at moderate temperatures and is very excellent as a very good intercalation type positive electrode A sample with a spinel structure is obtained. A sample of pure analytical reagent Co (NO 3 ) 2 is mixed with a sample of pure analytical reagent LiO 2 in a 2: 1 molar ratio to form a homogeneous mixture with three times the weight percent ammonium nitrate. . In order to obtain a better homogeneous mixture, this mixture is thoroughly ground with double distilled anhydrous diethylene carbonate (DEC). The mixture is heated to 300 ° C. and then continuously heated at 700 ° C. for 5 hours to obtain lithium cobaltate (LiCoO 2 ) as evidenced by X-ray analysis (FIG. 1b).
[0020]
The following examples are intended to illustrate the present invention and should not be construed to limit the technical scope of the present invention.
[0021]
Example 1: Production of LiCoO 2
LiO 2 of solid phase material, under controlled conditions, at a moderate temperature, are reacted with solid Co (NO 3) 2, just very good useful as excellent intercalation-type positive electrode A sample with a spinel structure is obtained. A sample of pure analytical reagent Co (NO 3 ) 2 is mixed with a sample of pure analytical reagent LiO 2 in a 2: 1 molar ratio to form a homogeneous mixture with 3 times weight percent of urea. . In order to obtain a better homogeneous mixture, this mixture is thoroughly ground with double distilled anhydrous diethylene carbonate (DEC). This mixture was heated at 300 ° C. for 3 hours and then continuously at 700 ° C. for 5 hours to obtain lithium cobaltate (LiCoO 2 ). Lithium cobaltate is evidenced by X-ray analysis (FIG. 1a).
[0023]
Example 2: Production of LiCoO 2
The solid-state material LiO 2 is reacted with solid Co (NO 3 ) 2 under controlled conditions at moderate temperatures and is very excellent as a very good intercalation type positive electrode A sample with a spinel structure is obtained. A sample of pure analytical reagent Co (NO 3 ) 2 is mixed with a sample of pure analytical reagent LiO 2 in a 2: 1 molar ratio to form a homogeneous mixture with three times the weight percent ammonium nitrate. . In order to obtain a better homogeneous mixture, this mixture is thoroughly ground with double distilled anhydrous diethylene carbonate (DEC). This mixture was heated to 300 ° C. and then continuously heated at 700 ° C. for 5 hours to obtain lithium cobaltate (LiCoO 2 ). Lithium cobaltate is evidenced by X-ray analysis (FIG. 1b).
[0025]
Example 3
[0026]
The pure and dried analytical reagent LiO 2 was mixed with the pure and dried analytical reagent Co (NO 3 ) 2 in a 1: 2 molar ratio using a mortar and pestle, and the mixture was then Further, 3 times the weight of urea was mixed and placed in an electric furnace. The mixture was first heated at 300 ° C. for 3 hours, followed by heating at 700 ° C. for 5 hours.
[0027]
[Table 1]
Example 4
[0029]
The pure and dried analytical reagent LiO 2 was mixed with the pure and dried analytical reagent Co (NO 3 ) 2 in a 1: 2 molar ratio using a mortar and pestle, and the mixture was then Further, 3 times by weight of ammonium nitrate was mixed. The final mixture was first heated at 300 ° C. for 3 hours, followed by heating at 700 ° C. for 5 hours.
[0030]
[Table 2]
Conclusion [0032]
1. Lithium oxide reacts with Co (NO 3 ) 2 at an equimolar ratio of 1: 2 to form LiCoO 2 .
2. Urea, ammonium nitrate and similar heat generating materials can be used as self-heating materials without significantly changing efficiency or product composition, and these materials are important for the formation of spinel structures.
3. The forming temperature is in the range of 650 ° C to 700 ° C.
4). The heating time is only about 8 hours.
[0033]
【The invention's effect】
The main effects of the present invention are as follows.
1. The production method of the present invention is a single-stage solid-state thermal reaction.
2. LiO 2, to form a LiCoO 2 high capacity positive electrode for intercalation, can be used for reaction with Co (NO 3) 2.
3. The heating time is only 8 hours, and therefore considerable heating time can be saved.
[Brief description of the drawings]
FIG. 1 is an X-ray diffraction pattern of lithium cobaltate obtained by the method according to the present invention.
Claims (8)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/IN2002/000066 WO2003080517A1 (en) | 2002-03-26 | 2002-03-26 | Solid state thermal synthesis of lithium cobaltate |
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| JP2005519840A JP2005519840A (en) | 2005-07-07 |
| JP3943081B2 true JP3943081B2 (en) | 2007-07-11 |
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| DE (1) | DE10296745T5 (en) |
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| CN112744871B (en) * | 2019-10-31 | 2022-12-13 | 天津国安盟固利新材料科技股份有限公司 | Lithium cobaltate cathode material and preparation method thereof |
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| AU2002249547A1 (en) | 2003-10-08 |
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