JP2018523902A - 二次電池用正極及びこれを含む二次電池 - Google Patents
二次電池用正極及びこれを含む二次電池 Download PDFInfo
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- JP2018523902A JP2018523902A JP2018509517A JP2018509517A JP2018523902A JP 2018523902 A JP2018523902 A JP 2018523902A JP 2018509517 A JP2018509517 A JP 2018509517A JP 2018509517 A JP2018509517 A JP 2018509517A JP 2018523902 A JP2018523902 A JP 2018523902A
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- positive electrode
- active material
- electrode active
- material layer
- conductive layer
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- Y10S977/902—Specified use of nanostructure
- Y10S977/932—Specified use of nanostructure for electronic or optoelectronic application
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Abstract
Description
本出願は、2015年11月30日付韓国特許出願第10−2015−0169150号及び2016年11月30日付韓国特許出願第10−2016−0161525号に基礎した優先権の利益を主張し、当該韓国特許出願の文献に開示されている全ての内容は、本明細書の一部として含まれる。
また、本発明が解決しようとする第2の技術的課題は、上記二次電池用正極の製造方法を提供することを目的とする。
正極集電体、
上記正極集電体の表面上に位置し、正極活物質及び第1炭素ナノチューブを含む多孔性正極活物質層、及び
上記正極活物質層が表面上に位置する導電層を含み、
上記導電層は、複数個の第2炭素ナノチューブによって形成された多孔性網状構造体を含み、正極活物質層の気孔度+10体積%以上の気孔度を有する二次電池用正極が提供される。
第2炭素ナノチューブを分散媒の中に添加して分散媒の表面上に第2炭素ナノチューブ膜が形成された導電層形成用組成物を準備する段階;及び
正極集電体の少なくとも一面に、正極活物質及び第1炭素ナノチューブを含む正極活物質層が形成された電極組み立て体を上記導電層形成用組成物に含浸した後、上記第2炭素ナノチューブ膜が正極活物質層表面上に位置するように電極組み立て体を持ち上げて導電層を形成する段階;を含む、上記二次電池用正極の製造方法が提供される。
正極集電体、
上記正極集電体の表面上に位置し、正極活物質及び第1炭素ナノチューブを含む多孔性正極活物質層、及び
上記正極活物質層が表面上に位置する導電層を含み、
上記導電層は、複数個の第2炭素ナノチューブによって形成された多孔性網状構造体を含み、正極活物質層の気孔度+10体積%以上の気孔度を有する二次電池用正極が提供される。
(上記化学式1で、M1はAl及びMnからなる群から選択されるいずれか一つまたは二つ以上の元素を含み、M2はW、Mo、Zr、Ti、Mg、Ta、Al、Fe、V、Cr、Ba、Ca、及びNbからなる群から選択されるいずれか一つまたは二つ以上の元素を含み、1.0≦a≦1.5、0<x≦0.5、0<y≦0.5、0<z≦0.02、0<x+y≦0.7のものであってもよく、より具体的には、1.0≦a≦1.2、0<x≦0.5、0<y≦0.5、0.0005≦z≦0.02、0<x+y≦0.7のものであってもよい)
第2炭素ナノチューブを分散媒の中に添加して分散媒の表面上に第2炭素ナノチューブ膜が形成された導電層形成用組成物を準備する段階(段階1);
正極集電体の少なくとも一面に、正極活物質及び第1炭素ナノチューブを含む正極活物質層が形成された電極組み立て体を上記導電層形成用組成物に含浸した後、上記第2炭素ナノチューブ膜が正極活物質層の表面上に位置するように電極組み立て体を持ち上げて導電層を形成する段階(段階2);を含む製造方法によって製造されることができる。
このような方法で形成する場合、従来の導電層スラリーを塗布する方法で導電層を形成する場合に比べて、より薄い厚さの導電層を形成することが可能であり、その結果、導電層内の物質伝達抵抗の増加を防止することができる。
また、上記バインダー及び導電材は、前述した正極と同じものであってもよい。
以下、実施例及び比較例における正極活物質層及び導電層の気孔度は、下記数式1及び2によってそれぞれ決定し、それぞれの物質の真密度を基準にして体積に換算し、所望の気孔度に該当する厚さで電極を圧延して調節した。
(正極集電体の製造)
Li(Ni0.6Mn0.2Co0.2)O2正極活物質(D50=11μm)、第1炭素ナノチューブ(単位体の長さ:3μm、直径:10nm、比表面積:300m2/g、バルク密度:0.13kg/m3のバンドル型炭素ナノチューブ)及びPVdFバインダーを98.02:0.4:1.58の重量比率でN−メチルピロリドン溶媒の中で混合して、正極形成用組成物(粘度:5000mPa・s)を製造し、これをアルミニウム集電体に塗布した後、130℃で乾燥して正極組み立て体を製造した(正極活物質層の気孔度:30体積%)。
第2炭素ナノチューブ(単位体の長さ:5μm、直径:10nm、比表面積:300m2/g、バルク密度:0.13kg/m3のバンドル型炭素ナノチューブ)0.05gをイソプロピルアルコール100mlの表面にゆっくり滴下した後、10分間超音波分散を行ってイソプロピルアルコール表面に第2炭素ナノチューブからなる3次元多孔性網状構造体を含む膜が形成された導電層形成用組成物を製造した。
上記製造された正極組み立て体を上記導電層形成用組成物に30秒間含浸させた後、上記第2炭素ナノチューブ膜が正極活物質層の表面上に位置するよう、電極組み立て体を0.15m/minの速度で3秒間ゆっくり持ち上げ、10Pa、80℃、6時間乾燥して正極活物質層の表面に導電層が形成された正極を製造した(対正極活物質層の導電層の厚さの比=1:0.002、活物質層の気孔度=30体積%、導電層の気孔度=56体積%、第1炭素ナノチューブ:第2炭素ナノチューブの重量比=1:0.17(図3参照)(下記表1参照)。
上記実施例1の正極集電体を製造する時、Li(Ni0.6Mn0.2Co0.2)O2の正極活物質(D50=11μm)、第1炭素ナノチューブ(単位体の長さ:3μm、直径:10nm、比表面積:300m2/g、バルク密度:0.13kg/m3のバンドル型炭素ナノチューブ)及びPVdFバインダーを98.26:0.2:1.54の重量比でN−メチルピロリドン溶媒の中で混合して製造した正極形成用組成物(粘度:5000mPa・s)を使うことを除いては、上記実施例1と同様の方法で行って正極を製造した(対正極活物質層の導電層の厚さの比=1:0.002、活物質層内の気孔度=30体積%、導電層の気孔度=56体積%、第1炭素ナノチューブ:第2炭素ナノチューブの重量比=1:0.34)(下記表1参照)。
上記実施例1の導電層形成用組成物を製造する時、第2炭素ナノチューブ(単位体の長さ:7μm、直径:9nm、比表面積:300m2/g、バルク密度:0.13kg/m3のバンドル型炭素ナノチューブ)0.9gをイソプロピルアルコール100mlの表面にゆっくり滴下した後、10分間超音波分散を行ってイソプロピルアルコール表面に第2炭素ナノチューブからなる3次元多孔性網状構造体を含む膜が形成された導電層形成用組成物を製造して使うことを除いては、上記実施例1と同様の方法で行って正極を製造した(対正極活物質層の導電層の厚さの比=1:0.005、活物質層内の気孔度=30体積%、導電層の気孔度=56体積%、第1炭素ナノチューブ:第2炭素ナノチューブの重量比=1:0.42)(下記表1参照)。
上記実施例1の導電層形成用組成物を製造する時、第2炭素ナノチューブ(単位体の長さ:3μm、直径:10nm、比表面積:300m2/g、バルク密度:0.13kg/m3のバンドル型炭素ナノチューブ)0.5gをイソプロピルアルコール100mlの表面にゆっくり滴下した後、10分間超音波分散を行ってイソプロピルアルコール表面に第2炭素ナノチューブからなる3次元多孔性網状構造体を含む膜が形成された導電層形成用組成物を使うことを除いて、上記実施例1と同様の方法で行って正極を製造した(対正極活物質層の導電層の厚さの比=1:0.001、活物質層内の気孔度=30体積%、導電層の気孔度=56体積%、第1炭素ナノチューブ:第2炭素ナノチューブの重量比=1:0.08)(下記表1参照)。
上記実施例1で正極活物質層の表面上に導電層を形成しないことを除いては、上記実施例1と同様の方法で行って正極を製造した(下記表1参照)。
上記実施例1で導電層を形成する時、導電層の気孔度を35%に下げたことを除いては、上記実施例1と同様の方法で行って正極を製造した(対正極活物質層の導電層の厚さの比=1:0.002、活物質層内の気孔度=30体積%、導電層の気孔度=35体積%、第1炭素ナノチューブ:第2炭素ナノチューブの重量比=1:0.1)(下記表1参照)。
上記実施例1で導電層を形成する時、炭素ナノチューブの含量を正極活物質層対比0.056の割合で高めて導電層内の気孔度と正極活物質層内の気孔度との差がほとんどないようにしたことを除いては、上記実施例1と同様の方法で行って正極を製造した(対正極活物質層の導電層の厚さの比=1:0.056、活物質層内の気孔度=30体積%、導電層の気孔度=30体積%、第1炭素ナノチューブ:第2炭素ナノチューブの重量比=1:4.7)(下記表1参照)。
上記実施例2で正極活物質層の表面上に導電層を形成しないことを除いては、上記実施例2と同様の方法で行って正極を製造した(正極活物質層内の気孔度=30体積%)(下記表1参照)。
(導電層形成用組成物の製造)
第2炭素ナノチューブ(単位体の長さ:5μm、直径:10nm、比表面積:300m2/g、バルク密度:0.13kg/m3のバンドル型炭素ナノチューブ)0.05gをイソプロピルアルコール100mlに混合して導電層形成用組成物を製造した。
上記実施例1で製造された正極組み立て体の表面に上記導電層形成用組成物を直接塗布した後、乾燥して導電層が表面にコーティングされた正極を製造した(図5参照)(対正極活物質層の導電層の厚さの比=1:0.02、活物質層内の気孔度=30体積%、導電層の気孔度=54体積%、第1炭素ナノチューブ:第2炭素ナノチューブの重量比=1:1.6)(下記表1参照)。
上記実施例1ないし4、比較例1ないし4及び参考例で製造した正極を利用してリチウム二次電池をそれぞれ製造した。
実験例1:率特性評価
上記実施例1ないし4、比較例1ないし4及び参考例で製造したそれぞれの正極を利用して製造したコインセル(Li金属の負極を使用)を25℃で0.1Cの定電流(CC)4.25Vになるまで充電し、以後4.25Vの定電圧(CV)で充電し、充電電流が0.05mAhになるまで1回目充電を行った。以後、20分間放置した後、0.1Cの定電流で3。0Vになるまで放電し、1サイクル目の放電容量を測定した。以後、2Cで放電条件を異にして率特性を評価した。その結果を下記図6に示した。
上記実施例1ないし4、比較例1ないし4及び参考例でのリチウム二次電池に対して、下記のような方法で抵抗特性を評価した。
2、12:正極活物質層
2a、12a:正極活物質
2b:第1炭素ナノチューブ
12b:炭素ナノチューブ
3:導電層
3a:第2炭素ナノチューブ
10、100:正極
Claims (13)
- 正極集電体、
上記正極集電体の表面上に位置し、正極活物質及び第1炭素ナノチューブを含む多孔性正極活物質層、及び
上記正極活物質層が表面上に位置する導電層を含み、
上記導電層は、複数個の第2炭素ナノチューブによって形成された多孔性網状構造体を含み、正極活物質層の気孔度+10体積%以上の気孔度を有する、二次電池用正極。 - 上記多孔性正極活物質層の気孔度は、10体積%ないし50体積%であり、
上記導電層の気孔度は、20体積%ないし60体積%である、請求項1に記載の二次電池用正極。 - 上記多孔性網状構造体は、正極活物質層内の第1炭素ナノチューブと繋がって電気的導電経路を形成する、請求項1に記載の二次電池用正極。
- 上記第1及び第2炭素ナノチューブは、それぞれ独立にバンドル型炭素ナノチューブである、請求項1に記載の二次電池用正極。
- 上記第1及び第2炭素ナノチューブは、それぞれ独立に炭素ナノチューブ単位体の直径が10nmないし100nmで、長さが3μmないし10μmである、請求項1に記載の二次電池用正極。
- 上記第1及び第2炭素ナノチューブは、それぞれ独立に比表面積が20m2/gないし2000m2/gである、請求項1に記載の二次電池用正極。
- 上記正極活物質の平均粒子直径(D50)が3μmないし20μmである、請求項1に記載の二次電池用正極。
- 上記正極活物質層:導電層の厚さの比は、1:0.001ないし1:0.05である、請求項1に記載の二次電池用正極。
- 上記正極活物質層:導電層の厚さの比は、1:0.001ないし1:0.01である、請求項8に記載の二次電池用正極。
- 上記正極活物質層:導電層の厚さの比は、1:0.001ないし1:0.005である、請求項8に記載の二次電池用正極。
- 上記第1炭素ナノチューブ:第2炭素ナノチューブの重量比は、1:0.08ないし1:0.42である、請求項1に記載の二次電池用正極。
- 第2炭素ナノチューブを分散媒の中に添加して分散媒の表面上に第2炭素ナノチューブ膜が形成された導電層形成用組成物を準備する段階;及び
正極集電体の少なくとも一面に、正極活物質及び第1炭素ナノチューブを含む正極活物質層が形成された電極組み立て体を上記導電層形成用組成物に含浸した後、上記第2炭素ナノチューブ膜が正極活物質層の表面上に位置するように電極組み立て体を持ち上げて導電層を形成する段階;を含む、請求項1に記載の二次電池用正極の製造方法。 - 請求項1ないし11のいずれか一項に記載の正極を含むリチウム二次電池。
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