JP6678358B2 - 骨格形成剤、これを用いた電極及び電極の製造方法 - Google Patents
骨格形成剤、これを用いた電極及び電極の製造方法 Download PDFInfo
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- JP6678358B2 JP6678358B2 JP2018044774A JP2018044774A JP6678358B2 JP 6678358 B2 JP6678358 B2 JP 6678358B2 JP 2018044774 A JP2018044774 A JP 2018044774A JP 2018044774 A JP2018044774 A JP 2018044774A JP 6678358 B2 JP6678358 B2 JP 6678358B2
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- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
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- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
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- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
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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
Description
Si+4.4Li++4.4e-→Li4.4Si ・・・・(式1)
0.5Si+0.5Al2O3+2.2Li++2.2e-
→0.5Li4.4Si+0.5Al2O3 ・・・・(式2)
D(Å)=0.9λ/(β×cosθ) ・・・・(式3)
(式中、Dは結晶粒の大きさ、λはX線管球の波長、βは結晶粒の大きさによる回折線の拡がり、θは回折角を示す)
[1.電極の製造方法]
まず、本実施形態の一例として、リチウム二次電池の電極の製造方法について説明する。なお、電極には負極と正極があるが、負極と正極は主に集電体及び活物質が異なるのみで製造方法は同様である。よって、負極の製造方法について説明し、正極の製造方法は適宜省略する。
Na2CO3+3SiO2→Na2O・3SiO2+CO2↑ ・・・・(式4)
2NaOH+3SiO2→Na2O・3SiO2+H2O ・・・・(式5)
上記の製造工程により製造された非水電解質二次電池用の負極は、銅箔の集電体と、その表面に活物質、導電助剤、バインダを含む活物質層とを備える。また、活物質層の表面は硬化した骨格形成剤によりコーティングされ、活物質層の内部にも硬化した骨格形成剤が存在している。また、活物質層の内部の骨格形成剤は、活物質と導電助剤とバインダを覆うようにこれらの隙間に存在している。また、活物質層の骨格形成剤の密度は一例として0.7mg/cm2であり、0.1mg〜3mg/cm2の範囲内にすることが好ましい。
上記したように本実施形態の骨格形成剤は、シロキサン結合を有するアルカリ金属ケイ酸塩であるNa2O・3SiO2の固形分濃度が7.5質量%であり、界面活性剤が0.09質量%で、残りは水である。なお、界面活性剤は必須ではないが、活物質層への親液性が向上し、骨格形成剤が活物質層に均一に浸透する。
以下、本実施形態において、骨格形成剤の固形分濃度や骨格密度など種々変更した実施例、それらの試験、結果及び効果について説明する。
(実施例1〜18および比較例1)
電極活物質にSi−C造粒体を用い、0.2C−rate、カットオフ電位0.01V〜1.2V(vs.Li+/Li)、30℃の条件のもと、骨格形成剤のNa2O・nSiO2の固形分濃度を0質量%〜20質量%、nの値を2.0、2.5、3.0に変化させた場合のサイクル寿命特性についての試験である。Si−C造粒体(D50=9.8μm)は、Si(D50=1.1μm)と人造黒鉛(D50=1μm)(Si:人造黒鉛=29:71質量%)および、造粒助剤からなる懸濁液を送液速度6g/min、噴霧圧0.1MPa、乾燥温度80〜180℃の条件でスプレードライすることで作製された。
実施例19〜36および比較例2は、活物質として、Si−C造粒体の組成が、Si:人造黒鉛=29:71質量%から、46:54質量%に代え、試験電極の容量密度を1.2mAh/cm2した他、先の試験(実施例1〜18および比較例1)と同様である。表2に、実施例19〜36および比較例2の骨格形成剤の固形分濃度、Na2O・nSiO2のnの値をそれぞれ示す。
実施例37〜40は、活物質がSi(D50=1.1μm)、骨格形成剤がLi0.05Na1.95O・3SiO2、試験電極の容量密度が3.0mAh/cm2にし、充放電試験は、0.1C−rate、カットオフ電位0.01V〜1.4V(vs.Li+/Li)の条件にした他、先の試験(実施例1〜18および比較例1)と同様である。表3に、実施例37〜40および比較例3の骨格形成剤の固形分濃度、電極の骨格密度をそれぞれ示す。なお、無機骨格形成剤は、Li2CO3、Na2CO3、およびSiO2からなる混合体を表3に示す組成になるように調合し、1000℃以上に加熱溶融して冷却後、水に溶解させて作製した。
(実施例41および実施例42)
実施例41は、電極活物質として、Si−C造粒体(Si:人造黒鉛=29:71質量%)を用い、骨格形成剤として、Na2O・nSiO2の固形分濃度を6質量%、nの値を2.5、骨格密度を0.84mg/cm2に調整した他の条件は実施例10と同様である。
(実施例43および比較例4)
骨格形成剤を用いた負極を適用した電池の安全性について試験を行った。試験方法は、電池モデルに釘を刺して、電池モデルの発煙や発火の状態について検討する釘刺し試験による。試験には、アルミラミネートケーシングに、負極、セパレータ、正極を複数積層して、電解液を封入した1.1Ahの電池モデルを用いた。正極(4.2mAh/cm2)は、LiNi0.33Co0.33Mn0.33O2とAB、PVdFからなるスラリーをアルミニウム箔(20μm)に塗工調圧後、160℃で熱処理することで作製された。負極(4.6mAh/cm2)は、人造黒鉛(D50=20μm)とAB、アクリル系バインダからなるスラリーを銅箔(10μm)に塗工調圧後、160℃で熱処理することで作製された。
(実施例43および比較例4)
実施例43および比較例4の電池で使用した負極の剥離試験を行った。剥離試験は、JIS K685に準拠し、負極の活物質層に粘着テープ(Scotch,No.845,Book Tape)を1kgローラーで圧着し、25℃環境下で引張り速度300mm/min、角度180°の条件で評価した。図16に、剥離試験後の実施例43および比較例4の負極および粘着テープの写真を示す。図16から明らかなように、骨格形成剤を使用しなかった比較例4の負極は、粘着テープに剥離した活物質層が付着しているが、骨格形成剤を使用した実施例43の負極は、粘着テープに活物質層がほぼ付着していない。剥離強度が向上することが示された。
(実施例44〜59および比較例5〜20)
表4に示した各種の負極活物質を用いて、骨格形成剤の有無における効果を比較した。実施例44〜59は、表4に示した負極活物質、AB、PVdFからなるスラリーを銅箔(10μm)に塗工調圧後、スプレーガンを用いて骨格形成剤を活物質層に被覆含浸し、160℃で熱処理することで作製された。電極スラリーの固形分比は、電極活物質が88質量%、ABが4質量%、PVdFが8質量%とした。
(実施例60〜63および比較例21〜24)
Si(1μm)と人造黒鉛(19μm)の混合物を負極活物質として用いた電極において、骨格形成の効果の有無を比較した。実施例60〜63は、表7に示した負極活物質、AB、PVdFからなるスラリーを銅箔(10μm)に塗工調圧後、スプレーガンを用いて骨格形成剤を活物質層に被覆含浸し、160℃で熱処理することで作製された。
各正極活物質を用いて、骨格形成剤の塗布量における効果を比較した。試験電極は、表9に示した正極活物質、AB、PVdFからなるスラリーをアルミニウム箔(20μm)に塗工調圧後、スプレーガンを用いて骨格形成剤を活物質層に含浸し、170℃で熱処理することで作製された。電極スラリーの固形分比は、電極活物質が90質量%、ABが5質量%、PVdFが5質量%とした。
実施例73〜81で用いた骨格形成剤は、Na2O・2.8SiO2と非イオン系界面活性剤(登録商標:トリトンX−100)からなる水溶液で、Na2O・3SiO2の固形分濃度が1.1質量%、界面活性剤の固形分濃度が0.03質量%のものを用いた。
(実施例82〜84および比較例21〜23)
実施例82は、電極容量を1.0mAh/cm2、骨格密度が0.06mg/cm2に変更した他、実施例74と同様である。実施例83は、電極容量を1.0mAh/cm2、骨格密度が0.07mg/cm2に変更した他、実施例76と同様である。実施例84は、電極容量を1.0mAh/cm2、骨格密度が0.11mg/cm2に変更した他、実施例81と同様である。比較例21は、電極容量を1.0mAh/cm2、骨格形成体を設けなかった他、実施例74と同様である。比較例22は、電極容量を1.0mAh/cm2、骨格形成体を設けなかった他、実施例76と同様である。比較例23は、電極容量を1.0mAh/cm2、骨格形成体を設けなかった他、実施例81と同様である。
以上の本実施形態によれば、次の効果を奏する。A2O・3SiO2(A=Na、Li)を含む骨格形成剤を電極に用いることで、耐熱性に優れ高強度で、サイクル寿命特性が向上した電極となる。また、強靱な集電体を必須とせず、集電体にしわや亀裂等の発生を抑制できる。また、不可逆容量の大きなバインダを用いる必要がない。また、活物質層の電子伝導性が高くても、内部短絡による発熱を低くできる。また、1000℃を超える耐熱性を有し、骨格形成剤が炭化しない。体積変化の激しい合金系材料と接着強度の低いバインダを用いた電極であっても、良好な寿命特性が得られる。また、高温の電解液と接触しても活物質層の膨潤が少ない。
[1.骨格形成剤と電極の構成]
次に、本発明の第2実施形態について説明する。第2実施形態と第1実施形態の違いは、主として骨格形成剤にセラミックスが含まれる点である。図12に、第2実施形態の電極断面イメージを示すが、第2実施形態の骨格形成剤は、耐アルカリ性に優れたセラミックス粉末あるいは固体電解質の粉末が含まれる。
次に、第2実施形態において、骨格形成剤の組成等、種々変更した実施例について説明する。
(実施例85〜87および比較例23)
表11に、実施例85〜87で用いた骨格形成剤の固形分組成を示す。また、骨格形成剤としてポリイミド(PI)を用いた電極を作製した(比較例23)。α−Al2O3は、レーザー回折・散乱式粒子径分布測定法によるメディアン径(D50)が0.95μmの粉末を用いた。骨格形成剤の固形分濃度は、Na2O・3SiO2とα−Al2O3の固形分を100質量%とした場合、10質量%とした。
表12に示すように、α−Al2O3の粒子径を変えて、骨格形成剤を電極本体の表面に塗工乾燥し、塗工性、新液性、結着性、発泡状態、凝集状態、沈降状態を観察した。骨格形成剤としては、Li0.05Na1.95O・3SiO2とα−Al2O3からなる水溶液である。骨格形成剤の固形分濃度は、Li0.05Na1.95O・3SiO2とα−Al2O3の固形分を100質量%とした場合、25質量%含まれている。なお、表12に示した無機粒子の粒径は、レーザー回折・散乱式粒子径分布測定法によるメディアン径(D50)を意味する。表12に示したように、第2実施形態において、セラミックスの粒子径は、0.2〜20μmの範囲内であることが好ましいことがわかる。
以上の本実施形態によれば、次の効果を奏する。第1実施形態で用いた骨格形成剤と耐アルカリ性に優れた粉末(D50=0.2〜20μm)を電極表面に塗布することで、活物質層に強固な骨格を形成することができるとともに、乾燥時の剥離やクラックの発生を抑制することができ、また、無機粒子同士の間隙により空孔が形成されて良好な電解液との親液性が得られる。また、セラミックス層がセパレータの代わりとなり、別途セパレータを用いずに、電池を構成することが可能となる。
<活物質造粒体の骨格形成>
(実施例88〜93)
骨格形成剤を適用したSi造粒体の製造方法についての試験である。
Si造粒体は、Si(D50=1μm)とABおよびVGCFおよびPIからなるからなる懸濁液を送液速度5g/min、噴霧圧0.1MPa、乾燥温度80〜180℃の条件でスプレードライし、D50=5〜8μmとなるように作製した。懸濁液の固形分比は、表13に示す通りである。
試験電極(4.0mAh/cm2)は、Si(1μm)、CB、PVdFバインダからなるスラリーを銅箔(40μm)に塗工調圧後、スプレーガンを用いて骨格形成剤を活物質層に被覆含浸し、300℃で熱処理することで作製された。骨格形成剤としては、リン酸アルミニウム(Al2O3・3P2O5)を水に溶解させ、固形分5質量%となるように調整した。電極の骨格密度は、片面当たり2.0mg/cm2である。負極スラリーの固形分比は、Siが90質量%、CBが4質量%、PVdFバインダが8質量%とした。
(比較例24)
骨格形成剤をバインダとして用いた試験である。バインダとしては、アルカリ金属ケイ酸塩(Li0.05Na1.95O・2.8SiO2)の固形分濃度が40質量%となるように水を加えて調整した。試験負極(2mAh/cm2)は、Si(D50=1μm)とカーボンブラック、無機バインダからなるスラリーを銅箔(10μm)に塗工し、150℃で熱処理した。電極スラリーの固形分比は、Siが19質量%、CBが4質量%、バインダが76質量%とした。
比較例25は、バインダとして、アルカリ金属ケイ酸塩から、第一リン酸アルミニウム塩(Al2O3・3P2O5)に変えた他、比較例24と同様である。なお、リン酸アルミニウム塩は、市販試薬(Aesar製)を用いた。
バインダとして、アルカリ金属ケイ酸塩(Li0.05Na1.95O・2.8SiO2)とα−Al2O3(D50=3μm)を50:50質量%となるように混合し、この混合体の固形分濃度が40質量%となるように水を加えて調整した。その他の条件としては、比較例24と同様である。
バインダとして、リン酸アルミニウム塩(Al2O3・3P2O5)とα−Al2O3(D50=3μm)を50:50質量%となるように混合し、この混合体の固形分濃度が40質量%となるように水を加えて調整した。その他の条件としては、比較例25と同様である。
(参考例3)
骨格形成剤が電極に浸透しているかを確認した試験である。模擬電極は、Al2O3(D50=9μm)、AB、PVdFバインダからなるスラリーを銅箔(10μm)に塗工調圧後、スプレーガンを用いて骨格形成剤を活物質層に被覆含浸し、150℃で熱処理することで作製された。骨格形成剤としては、アルカリ金属ケイ酸塩(Na2O・3SiO)を水に溶解させ、固形分8質量%となるように調整した。なお、界面活性剤は加えていない。模擬電極スラリーの固形分比は、α−Al2O3が85質量%、CBが5質量%、PVdFバインダが10質量%とした。
参考例4は、比較として、骨格形成剤を被覆含浸しなかった電極である他、参考例3と同じである。図20に、参考例3と参考例4のグロー放電発光分光分析(GDS)結果を示す。GDS測定条件としては、測定径4mmφ、Neガス圧力2000Paとした。測定波長はHでは121nm、Fでは685nm、Oでは130nm、Cでは156nm、Alでは396nm、Siでは251nmとした。横軸の時間は、スパッタ処理した時間で、活物質層の深さ方向(電極表面から集電体への方向)に相当する指標である。縦軸の強度は、発光強度で、元素の含有率に相当する指標である。図20から明らかなように、参考例4ではSiの存在が確認できないのに対して、参考例3は、Siの存在が表面から内部まで一定ではないものの、深層にSiが存在していることが確認できた。この結果から、骨格形成剤を電極表面に塗布することで、骨格形成剤が活物質層内部まで浸透しうることが証明された。
Claims (14)
- アルカリ金属と合金化が可能な活物質又はアルカリ金属イオンを吸蔵することが可能な活物質と、バインダと、を含む非水電解質二次電池の電極における活物質層の骨格形成に用いる骨格形成剤であって、
成分にシロキサン結合を有する非晶質のケイ酸塩、又は、アルミノリン酸結合を有する非晶質のリン酸塩を含む、骨格形成剤。 - さらに、界面活性剤を含む、
請求項1に記載の骨格形成剤。 - 前記界面活性剤は、0.001質量%以上5.0質量%以下である、
請求項2に記載の骨格形成剤。 - 前記ケイ酸塩は、
一般式A2O・nSiO2で表される非晶質構造であり、
Aは、Li、Na、K、トリエタノールアンモニウム基、テトラメタノールアンモニウム基、テトラエタノールアンモニウム基、グラニジン基の少なくともいずれか1種であり、
nが、1.6以上3.9以下である、
請求項1乃至請求項3のいずれか1項に記載の骨格形成剤。 - 前記一般式のAが、LiまたはNaであり、
nが、2.0以上3.5以下である、
請求項4に記載の骨格形成剤。 - 前記ケイ酸塩の固形分濃度が0.1質量%以上30質量%以下である、
請求項1乃至請求項5のいずれか1項に記載の骨格形成剤。 - さらに、耐アルカリ性又は耐酸性の無機粒子を含む、
請求項1乃至請求項6のいずれか1項に記載の骨格形成剤。 - 前記ケイ酸塩及び前記無機粒子を含む固形分の合計を100質量%とした場合に、
前記ケイ酸塩が5質量%以上80質量%以下であり、
前記無機粒子が20質量%以上95質量%以下であり、
前記無機粒子のメディアン径が0.2μm以上20μm以下である、
請求項7に記載の骨格形成剤。 - 請求項1乃至請求項8のいずれか1項に記載の骨格形成材が、
少なくとも活物質層の表面に存在する、電極。 - 請求項1乃至請求項8のいずれか1項に記載の骨格形成材が、
少なくとも活物質層内に存在する、電極。 - 非水電解質二次電池の電極の製造方法であって、
アルカリ金属と合金化が可能な活物質又はアルカリ金属イオンを吸蔵することが可能な活物質と、バインダと、導電助剤とを混練して活物質層となる電極材料を製造し、線状、棒状、板状、箔状、多孔状の集電体の表面に電極材料を塗工して電極を製造する工程を含み、
成分にシロキサン結合を有する非晶質のケイ酸塩、又は、アルミノリン酸結合を有する非晶質のリン酸塩を含む骨格形成剤を、前記電極の活物質層の表面に塗工する工程Aと、前記電極を乾燥する工程Bと、を備える、
電極の製造方法。 - 前記工程Aにおいて、前記活物質層の表面から内部に前記骨格形成剤が浸透する、
請求項11に記載の電極の製造方法。 - 前記工程Aは、
前記骨格形成剤を入れた槽に、前記電極を含浸する工程である、
請求項11又は請求項12に記載の電極の製造方法。 - 前記骨格形成剤におけるケイ酸塩の固形分濃度が、0.1乃至30質量部であり、
前記工程Bは、60℃以上の温度で熱処理する工程である、
請求項11乃至請求項13のいずれか1項に記載の電極の製造方法。
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