JP6811175B2 - リチウムイオン二次電池 - Google Patents
リチウムイオン二次電池 Download PDFInfo
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- JP6811175B2 JP6811175B2 JP2017521776A JP2017521776A JP6811175B2 JP 6811175 B2 JP6811175 B2 JP 6811175B2 JP 2017521776 A JP2017521776 A JP 2017521776A JP 2017521776 A JP2017521776 A JP 2017521776A JP 6811175 B2 JP6811175 B2 JP 6811175B2
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- negative electrode
- graphite
- mass
- positive electrode
- ion secondary
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Description
<正極の作製>
正極活物質であるLiCoO2:96.5質量部と、バインダであるP(VDF−CTFE)を10質量%の濃度で含むNMP溶液:20質量部と、導電助剤であるアセチレンブラック:1.5質量部とを、二軸混練機を用いて混練し、更にNMPを加えて粘度を調節して、正極合剤含有ペーストを調製した。このペーストを厚みが15μmのアルミニウム箔の片面または両面に塗布し、120℃で12時間の真空乾燥を行って、アルミニウム箔の片面または両面に正極合剤層を形成し、プレス処理を行い、所定の大きさで切断して、帯状の正極を得た。なお、アルミニウム箔への正極合剤含有ペーストの塗布の際には、アルミニウム箔の一部が露出するようにし、アルミニウム箔の両面に正極合剤含有ペーストを塗布したものでは、表面で塗布部とした箇所は裏面も塗布部とした。得られた正極の正極合剤層の厚み(アルミニウム箔の両面に正極合剤層を形成したものでは、片面あたりの厚み)は、55μmであった。
表1に示す黒鉛A−1(表面を非晶質炭素で被覆していない黒鉛):25質量%と、黒鉛B−1(黒鉛からなる母粒子の表面を、ピッチを炭素源とした非晶質炭素で被覆した黒鉛):25質量%と、SiO表面を炭素材料で被覆した複合体Si−1(材料S、平均粒径が8μm、比表面積が7.9m2/gで、複合体における炭素材料の量が20質量%):50質量%とを、V型ブレンダーで12時間混合し、負極活物質を得た。
変性ポリブチルアクリレートの樹脂バインダ:3質量部と、ベーマイト粉末(平均粒径1μm):97質量部と、水:100質量部とを混合し、多孔質層(II)形成用スラリーを作製した。このスラリーを、厚さ12μmのリチウムイオン電池用ポリエチレン製微多孔膜〔多孔質層(I)〕の片面に塗布、乾燥をした。多孔質層(I)の片面にベーマイトを主体として含む多孔質層(II)を形成したセパレータを得た。なお、多孔質層(II)の厚みは3μmであり、ベーマイトの体積含有率は90体積%であった。
正極集電体の片面に正極合剤層を形成した電池用正極2枚、正極集電体の両面に正極合剤層を形成した電池用正極14枚、および負極集電体の両面に負極合剤層を形成した電池用負極15枚を用いて積層電極体を形成した。積層電極体では、上下の両端を正極集電体の片面に正極合剤層を形成した電池用正極として、それぞれの集電体が外側を向くように配置し、それらの間に負極集電体の両面に負極合剤層を形成した電池用負極と正極集電体の両面に正極合剤層を形成した電池用正極とを交互に配置し、各正極と各負極との間にはセパレータを介在させ、正極同士のタブ部、負極同士のタブ部を、それぞれ溶接して積層電極体を作製した。そして、前記積層電極体が収まるように窪みを形成した厚み:0.15mm、幅:34mm、高さ:50mmのアルミニウムラミネートフィルムの、前記窪みに前記積層電極体を挿入し、その上に前記と同じサイズのアルミニウムラミネートフィルムを置いて、両アルミニウムラミネートフィルムの3辺を熱溶着した。そして、両アルミニウムラミネートフィルムの残りの1辺から非水電解液(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3:7の混合溶媒に、LiPF6を1mol/lの濃度で溶解させ、更にビニレンカーボネートを3質量%となる量で添加した溶液)を注入した。その後、両アルミニウムラミネートフィルムの前記残りの1辺を真空熱封止して、図3に示す外観で、図4に示す断面構造のリチウムイオン二次電池を作製した。
表1に示す材料Sおよび黒鉛を、表6、表8、または表10および表11に示す質量比率で混合した負極活物質を用いた以外は、すべて実施例1と同様にしてリチウムイオン二次電池を作製した。
実施例1で作製した負極合剤含有ペーストを、一方の面から他方の面へ貫通する貫通孔を有した銅箔(厚みが10μm、貫通孔の直径が0.3mm、貫通孔間のピッチが0.8mm)の両面に塗布し乾燥を行って、銅箔の両面に負極合剤層を形成し、プレス処理を行って負極合剤層の密度を1.4g/cm3に調整した後に所定の大きさで切断して、帯状の負極とし、これを実施例1と同様に打ち抜いて、負極合剤層を集電体の両面に有する電池用負極を得た。厚さ30μmのLi箔を打ち抜き、この負極の片側の負極合剤層の表面に、表12に示した量のLi箔を貼付した。そして、負極合剤層を集電体の両面に有する電池用負極を、前記のものに変更した以外は、実施例1と同様にしてリチウムイオン二次電池を作製した。
正極活物質であるLiCoO2(80質量部)およびLi1.02Ni0.5Co0.2Mn0.3O2(20質量部)と、バインダであるP(VDF−CTFE)をNMPに溶解させた溶液20質量部と、導電助剤である人造黒鉛1質量部およびケッチェンブラック1質量部とを、二軸混練機を用いて混練し、更にNMPを加えて粘度を調節して、正極合剤含有ペーストを調製した。このペーストを用いた以外は、実施例1と同様の手法で正極を作製した。以下、実施例1と同様にしてリチウムイオン二次電池を得た。
黒鉛A−1:50質量%と黒鉛B−1:50質量%とを、V型ブレンダーで12時間混合し、負極活物質を得た。この負極活物質を使用した以外は、実施例1と同様にして負極を作製した。この負極を、負極合剤層にLi箔を貼付しない状態で使用した以外は、実施例1と同様にしてリチウムイオン二次電池を作製した。
黒鉛A−1:50質量%と黒鉛B−1:50質量%とを、V型ブレンダーで12時間混合し、負極活物質を得た。この負極活物質を使用した以外は、実施例1と同様にして負極を作製した。この負極を用いた以外は、実施例1と同様にしてリチウムイオン二次電池を作成した。
負極合剤層を有する面に、Li箔を貼付しなかったこと以外は、すべて実施例1と同様にしてリチウムイオン二次電池を作製した。
セパレータとしてリチウムイオン二次電池用のPE製セパレータ(厚み16μm)を用いたこと以外は、すべて実施例1と同様にしてリチウムイオン二次電池を作製した。
負極合剤層を有する面に、Li箔を貼付しなかったこと以外は、すべて実施例2と同様にしてリチウムイオン二次電池を作製した。
負極合剤層を有する面に、Li箔を貼付しなかったこと以外は、すべて実施例9と同様にしてリチウムイオン二次電池を作製した。
セパレータとしてリチウムイオン二次電池用のPE製セパレータ(厚み16μm)を用いたこと以外は、すべて実施例2と同様にしてリチウムイオン二次電池を作製した。
セパレータとしてリチウムイオン二次電池用のPE製セパレータ(厚み16μm)を用いたこと以外は、すべて実施例9と同様にしてリチウムイオン二次電池を作製した。
60℃の恒温槽で24時間保管したリチウムイオン二次電池を、0.1Cの放電電流レートで電圧が2.0Vに達するまで放電した。その後、グローブボックス内でアルミラミネートを解体し、正極のみを取り出した。取り出した正極をジエチルカーボネートで洗浄したのち、正極合剤層を掻き出し、前述したICP法により、LiとLi以外の金属Mとの組成比率(モル比率Li/M)を算出した。
実施例および比較例のリチウムイオン二次電池(上述したLi/M算出用とは別のもの)を、25℃の恒温槽内に5時間静置し、その後、各電池について、0.5Cの電流値で4.4Vまで定電流充電し、引き続いて4.4Vで定電圧充電し(定電流充電と定電圧充電との総充電時間が2.5時間)、その後に0.2Cの定電流で2.0V(比較例1の電池は2.75V)まで放電を行って、初回放電容量を求めた。次に、各電池について、1Cの電流値で4.4Vまで定電流充電し、引き続いて4.4Vの定電圧で電流値が0.05Cになるまで充電した後に、1Cの電流値で2.0V(比較例1の電池は2.75V)まで放電する一連の操作を1サイクルとして、これを500回サイクル行った。そして、各電池について、前記の初回放電容量測定時と同じ条件で定電流−定電圧充電および定電流放電を行って、放電容量を求めた。そして、これらの放電容量を初回放電容量で除した値を百分率で表して、サイクル容量維持率を算出した。なお、初回放電容量は、比較例1の放電容量を100%とした場合の比率として示す。
11 正極合剤層
12 正極集電体
13 タブ部
20 負極
21 負極合剤層
22 負極集電体
23 タブ部
100 リチウムイオン二次電池
101 金属ラミネートフィルム外装体
102 積層電極体
103 正極外部端子
104 負極外部端子
Claims (5)
- 正極、負極、セパレータおよび非水電解液を少なくとも外装体に装填したリチウムイオン二次電池において、
前記負極は、負極活物質を主体とした負極合剤層を、負極集電体の少なくとも一方の面に有しており、かつ前記負極活物質として、SiOx(ただし、0.5≦x≦1.5である)を含む材料Sと、下記の平均粒子径が15μm以上25μm以下の黒鉛Aと、下記の平均粒子径が8μm以上15μm未満であり、黒鉛粒子の表面が非晶質炭素で被覆されている黒鉛Bとを含有しており、
前記負極中に含まれる全負極活物質の合計を100質量%とした場合、前記黒鉛Aと前記黒鉛Bとの合計比率(A+B)が20質量%以上99質量%以下であり、前記黒鉛Bに対する前記黒鉛Aの質量比率(A/B)が0.5以上4.5以下であり、
前記セパレータは、熱可塑性樹脂を主体とする多孔質層(I)と、耐熱温度が150℃以上のフィラーを主体として含む多孔質層(II)とを有しており、
前記正極は、正極活物質として、LiとLi以外の金属Mとで構成される金属酸化物を含有しており、
0.1Cの放電電流レートで電圧が2.0Vに達するまで放電した時の、前記正極活物質に含まれるLiとLi以外の金属Mとのモル比率(Li/M)が0.9〜1.05であることを特徴とするリチウムイオン二次電池。
前記黒鉛Aの平均粒子径および前記黒鉛Bの平均粒子径は、粒度分布の小さい粒子から積分体積を求める場合の体積基準の積算分率における50%径の値であるメディアン径である。 - 前記負極中に含まれる全負極活物質の合計を100質量%とした場合、前記材料Sの含有率が少なくとも20質量%であり、前記黒鉛Aと前記黒鉛Bとの合計比率(A+B)が80質量%以下である請求項1に記載のリチウムイオン二次電池。
- 前記負極集電体は、一方の面から他方の面へ貫通する貫通孔を有している請求項1または2に記載のリチウムイオン二次電池。
- 前記外装体が、金属ラミネートフィルム外装体である請求項1〜3のいずれかに記載のリチウムイオン二次電池。
- 前記正極と前記負極とは、前記セパレータを介して積層された電極体を形成している請求項1〜4のいずれかに記載のリチウムイオン二次電池。
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