JP2020113532A - 電極合材用液体組成物、電極の製造方法及び電気化学素子の製造方法 - Google Patents
電極合材用液体組成物、電極の製造方法及び電気化学素子の製造方法 Download PDFInfo
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- JP2020113532A JP2020113532A JP2019200162A JP2019200162A JP2020113532A JP 2020113532 A JP2020113532 A JP 2020113532A JP 2019200162 A JP2019200162 A JP 2019200162A JP 2019200162 A JP2019200162 A JP 2019200162A JP 2020113532 A JP2020113532 A JP 2020113532A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
Description
本実施形態の電極合材用液体組成物(以下、液体組成物という)は、活物質A、分散媒B及び重合性化合物Cを含み(図1参照)、必要に応じて、導電助剤、分散剤等をさらに含んでいてもよい。
活物質としては、正極活物質又は負極活物質を用いることができる。
分散媒としては、活物質を分散させることが可能であれば、特に制限はないが、水、エチレングリコール、プロピレングリコール等の水性分散媒、N−メチル−2−ピロリドン、2−ピロリドン、シクロヘキサノン、酢酸ブチル、メシチレン、2−n−ブトキシメタノール、2−ジメチルエタノール、N,N−ジメチルアセトアミド等の有機分散媒が挙げられる。
重合性化合物は、重合開始剤又は触媒と併用することが好ましい。
導電助剤としては、例えば、ファーネス法、アセチレン法、ガス化法等により製造されている導電性カーボンブラックや、カーボンナノファイバー、カーボンナノチューブ、グラフェン、黒鉛粒子等の炭素材料を用いることができる。炭素材料以外の導電助剤としては、例えば、アルミニウム等の金属粒子、金属繊維を用いることができる。なお、導電助剤は、予め活物質と複合化されていてもよい。
分散剤としては、分散媒中の活物質、導電助剤の分散性を向上させることが可能であれば、特に制限はないが、例えば、ポリカルボン酸系分散剤、ナフタレンスルホン酸ホルマリン縮合系分散剤、ポリエチレングリコール、ポリカルボン酸部分アルキルエステル系分散剤、ポリエーテル系分散剤、ポリアルキレンポリアミン系分散剤等の高分子型分散剤、アルキルスルホン酸系分散剤、四級アンモニウム塩系分散剤、高級アルコールアルキレンオキシド系分散剤、多価アルコールエステル系分散剤、アルキルポリアミン系分散剤等の界面活性剤型分散剤、ポリリン酸塩系分散剤等の無機型分散剤等が挙げられる。
本実施形態の電極の製造方法は、本実施形態の液体組成物を、電極基体上に塗布する工程を含む。
図3に、本実施形態の負極の一例を示す。
図4に、本実施形態の負極の製造方法の一例を示す。
図7に、本実施形態の正極の一例を示す。
正極20の製造方法は、正極基体21上に、正極合材22用液体組成物を吐出する以外は、負極10の製造方法と同様である。
本実施形態の電気化学素子の製造方法は、本実施形態の電極の製造方法を用いて電極を製造する工程を含む。
図8に、本実施形態の電気化学素子に用いる電極素子の一例を示す。
セパレータ30は、負極15と正極25の短絡を防ぐために、必要に応じて、負極15と正極25の間に設けられている。
図9に、本実施形態の電気化学素子の一例を示す。
電解質水溶液を構成する電解質塩としては、水酸化ナトリウム、水酸化カリウム、塩化ナトリウム、塩化カリウム、塩化アンモニウム、塩化亜鉛、酢酸亜鉛、臭化亜鉛、ヨウ化亜鉛、酒石酸亜鉛、過塩化亜鉛等が挙げられる。
非水電解質としては、固体電解質又は非水電解液を使用することができる。
非水溶媒としては、特に制限はなく、例えば、非プロトン性有機溶媒を用いることが好ましい。
等を用いることができる。
電解質塩としては、イオン伝導度が高く、非水溶媒に溶解することが可能であれば、特に制限はない。
電気化学素子の用途としては、特に制限はなく、例えば、ノートパソコン、ペン入力パソコン、モバイルパソコン、電子ブックプレーヤー、携帯電話、携帯ファックス、携帯コピー、携帯プリンター、ヘッドホンステレオ、ビデオムービー、液晶テレビ、ハンディークリーナー、ポータブルCD、ミニディスク、トランシーバー、電子手帳、電卓、メモリーカード、携帯テープレコーダー、ラジオ、バックアップ電源、モーター、照明器具、玩具、ゲーム機器、時計、ストロボ、カメラ等が挙げられる。
実施例で用いた分散媒に活物質を分散させた後、レーザ回折式粒度分布測定装置マスターサイザー3000(マルバーン製)を用いて、25℃で活物質の粒度分布を計測した。
B型粘度計(コーンプレート型粘度計)にNo.CPA−40Zのロータを装着して、回転数100rpm、温度25℃の条件で、液体組成物の粘度を測定した。
粘着皮膜剥離解析装置VPA−3(協和界面科学製)を用いて、電極合材の剥離強度を測定した(ピール強度試験法)。具体的には、作製した電極を、幅1cm×長さ10cmに切断した試験片の電極合材側の表面にセロハンテープを貼り付けた後、剥離速度30mm/分、剥離角度90°の条件で、試験片の一端からセロハンテープを100mm引き剥がし、その時の応力を測定した。このような測定を10回実施し、その加重平均を求めた。
充放電測定装置TOSCAT3001(東洋システム製)を用いて、正極の単位面積当たりの容量を測定した。室温(25℃)において、非水系蓄電素子に0.1mA/cm2の定電流で充電終止電圧4.2Vまで充電した後、0.1mA/cm2の定電流で2.5Vまで放電して初期充放電を実施した。次に、非水系蓄電素子に0.1mA/cm2の定電流で4.2Vまで充電した後、0.1mA/cm2の定電流で2.5Vまで放電する充放電サイクルを2回実施し、正極の単位面積当たりの容量を測定した。
充放電測定装置TOSCAT3001(東洋システム製)を用いて、正極の単位面積当たりの容量を測定した。室温(25℃)において、非水系蓄電素子に0.1mA/cm2の定電流で充電終止電圧3.8Vまで充電した後、0.1mA/cm2の定電流で2.7Vまで放電して初期充放電を実施した。次に、非水系蓄電素子に0.1mA/cm2の定電流で3.8Vまで充電した後、0.1mA/cm2の定電流で2.7Vまで放電する充放電サイクルを2回実施し、正極の単位面積当たりの容量を測定した。
五酸化バナジウム、水酸化リチウム、リン酸、スクロース、水を混合して沈殿を生成させた後、粉砕して、リン酸バナジウム粒子の前駆体を得た。次に、窒素雰囲気下、900℃で、リン酸バナジウムの前駆体を焼成し、炭素含有量3質量%のリン酸バナジウムリチウム(LVP)(正極活物質1)を得た。正極活物質1は、モード径が10μmであった。さらに、ジェットミルを用いて、正極活物質1を解砕して、正極活物質2を得た。正極活物質2は、モード径が0.7μmであった。
正極活物質3として、ニッケル系正極活物質(NCA)(JFEミネラル製)を用いた。正極活物質3は、モード径が12μmであった。さらに、ジェットミルを用いて、正極活物質3を解砕して、正極活物質4を得た。正極活物質4は、モード径が1.5μmであった。
正極活物質5として、リン酸鉄リチウム(LFP)(TATUNG FINE CHEMICALS製)を用いた。正極活物質5は、モード径が8.0μmであった。さらに、ビーズミルを用いて、正極活物質5を解砕して、正極活物質6を得た。正極活物質6は、モード径が1.0μmであった。
充放電測定装置TOSCAT3001(東洋システム製)を用いて、負極の単位面積当たりの容量を測定した。室温(25℃)において、非水系蓄電素子に0.1mA/cm2の定電流で充電終止電圧1.0Vまで充電した後、0.1mA/cm2の定電流で2.0Vまで放電して初期充放電を実施した。次に、非水系蓄電素子に0.1mA/cm2の定電流で1.0Vまで充電した後、0.1mA/cm2の定電流で2.0Vまで放電する充放電サイクルを2回実施し、負極の単位面積当たりの容量を測定した。
負極活物質1として、チタン酸リチウム(LTO)(石原産業製)を用いた。負極活物質1は、モード径が2.0μmであった。さらに、ビーズミルを用いて、負極活物質1を解砕して、負極活物質2を得た。負極活物質2は、モード径が1.0μmであった。
エチレンカーボネート(EC)/ジメチルカーボネート(DMC)/エチルメチルカーボネート(EMC)の混合溶媒(質量比1:1:1)に、1.5mol/LのLiPF6を溶解させ、非水電解液1(20mL)を得た。
正極活物質1(30質量%)、カーボンブラック(1質量%)、ペンタエリトリトールテトラアクリラート(PETTA)(東京化成工業製)(0.3質量%)、ヘキサメチレンジアミン(HMD)(東京化成工業製)(0.7質量%)、触媒ジアザビシクロウンデセン(DBU)(東京化成工業製)(0.01質量%)、N−メチルピロリドン(NMP)(富士フイルム和光純薬製)(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が15.3mPa・sであった。
正極活物質2(30質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMPとプロピレングリコール(PG)(富士フイルム和光純薬製)の混合分散媒(質量比7:3)(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が11.2mPa・sであった。
正極活物質2(30質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMPと2−ピロリドン(富士フイルム和光純薬製)の混合分散媒(質量比7:3)(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が10.5mPa・sであった。
正極活物質2(40質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMPと2−ピロリドンの混合分散媒(質量比7:3)(57.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が15.6mPa・sであった。
正極活物質2(20質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMPと2−ピロリドンの混合分散媒(質量比7:3)(77.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が9.7mPa・sであった。
正極活物質3(30質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMP(67.99質量%)を混合し、液体組成物を得た。液体組成物は、粘度が13.8mPa・sであった。
正極活物質4(30質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMPとPGの混合分散媒(質量比7:3)(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が12.4mPa・sであった。
正極活物質5(30質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMP(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が15.1mPa・sであった。
正極活物質6(30質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMPとPGの混合分散媒(質量比7:3)(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が14.8mPa・sであった。
正極活物質1(30質量%)、カーボンブラック(1質量%)、ペンタエリスリトールトリアクリレート(PETA)(ダイセル・オルネクス製)(0.4質量%)、HMD(0.6質量%)、触媒DBU(0.01質量%)、NMPとPGの混合分散媒(質量比7:3)(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が13.2mPa・sであった。
正極活物質2(30質量%)、カーボンブラック(1質量%)、PETA(0.4質量%)、HMD(0.6質量%)、触媒DBU(0.01質量%)、NMPとPGの混合分散媒(質量比7:3)(67.99質量%)を混合し、正極合材用液体組成物を作製した。正極合材用液体組成物の粘度は、12.1mPa・sであった。
正極活物質2(30質量%)、カーボンブラック(1質量%)、IRR 214−K(トリシクロデカンジメタノールジアクリレート)(ダイセル・オルネクス製)(3.3質量%)、重合開始剤V−65(2,2'−アゾビス(2,4−ジメチルバレロニトリル))(富士フイルム和光純薬製)(0.033質量%)、ジプロピレングリコールモノメチルエーテル(GPGME)(65.667質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が15.1mPa・sであった。
正極活物質2(30質量%)、カーボンブラック(1質量%)、PETA(3.3質量%)、重合開始剤V−65(0.033質量%)、GPGME(65.667質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が17.1mPa・sであった。
正極活物質4(30質量%)、カーボンブラック(1質量%)、IRR 214−K(ダイセル・オルネクス製)(1質量%)、重合開始剤V−65(0.01質量%)、GPGME(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が14.9mPa・sであった。
正極活物質4(30質量%)、カーボンブラック(1質量%)、PETA(1質量%)、重合開始剤V−65(0.01質量%)、GPGME(67.99質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が16.8mPa・sであった。
負極活物質1(30質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(触媒量)、NMP(68質量%)を混合し、負極合材用液体組成物を得た。負極合材用液体組成物は、粘度が16.6mPa・sであった。
負極活物質2(30質量%)、カーボンブラック(1質量%)、PETTA(0.3質量%)、HMD(0.7質量%)、触媒DBU(0.01質量%)、NMPとPGの混合分散媒(質量比7:3)(67.99質量%)を混合し、負極合材用液体組成物を得た。負極合材用液体組成物は、粘度が15.4mPa・sであった。
正極活物質1(30質量%)、カーボンブラック(1質量%)、ポリフッ化ビニリデン(PVDF)(1質量%)、NMP(68質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が1092mPa・sであった。
正極活物質1(30質量%)、カーボンブラック(1質量%)、PVDF(0.5質量%)、NMP(68.5質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が611mP・sであった。
正極活物質1(30質量%)、カーボンブラック(1質量%)、NMP(69質量%)を混合し、正極合材用液体組成物を得た。正極合材用液体組成物は、粘度が10.2mPa・sであった。ホットプレートで120℃に加熱したアルミニウム箔(正極基体)上に、バーコート法により、正極合材用液体組成物を塗布し、単位面積当たりの正極活物質量が2.1mg/cm2である正極を得た。正極は、正極合材の剥離強度が0.002Nであった。
電極の単位面積当たりの容量を測定した実施例1及び実施例12の非水系蓄電素子に1mA/cm2の電流で放電した以外は、電極の単位面積当たりの容量と同様にして、電極の単位面積当たりの容量を測定した。その結果、式
(1mA/cm2の電流で放電した際の容量)/(0.1mA/cm2の電流で放電た際の容量)
で表される値は、実施例1の正極が95.1%であり、実施例12の正極が97.2%であった。次に、実施例1及び実施例12の非水系蓄電素子に5mA/cm2の電流で放電した以外は、電極の単位面積当たりの容量と同様にして、電極の単位面積当たりの容量を測定した。その結果、式
(5mA/cm2の電流で放電した際の容量)/(0.1mA/cm2の電流で放電した際の容量)
で表される値は、実施例1の正極は87.3%であり、実施例12の正極が94.2%であった。
B 分散媒
C 重合性化合物
C' バインダー
D 電極基体
1 電気化学素子
10、15 負極
11 負極基体
12 負極合材層
12A 液体組成物
20、25 正極
21 正極基体
22 正極合材層
30 セパレータ
40 電極素子
41、42 引き出し線
51 電解質層
52 外装
300、300' 液体吐出装置
306 液体吐出ヘッド
Claims (9)
- 活物質、分散媒及び重合性化合物を含み、
25℃における粘度が液体吐出ヘッドから吐出することが可能な粘度であることを特徴とする電極合材用液体組成物。 - 25℃における粘度が50mPa・s以下であることを特徴とする請求項1に記載の電極合材用液体組成物。
- 前記活物質は、アルカリ金属イオンを挿入又は放出することが可能な材料であることを特徴とする請求項1又は2に記載の電極合材用液体組成物。
- 前記活物質の含有量が20質量%以上であることを特徴とする請求項1乃至3のいずれか一項に記載の電極合材用液体組成物。
- 前記活物質は、最大粒子径が前記液体吐出ヘッドのノズル径以下であることを特徴とする請求項1乃至4のいずれか一項に記載の電極合材用液体組成物。
- 前記活物質は、モード径が3μm以下であることを特徴とする請求項1乃至5のいずれか一項に記載の電極合材用液体組成物。
- 前記分散媒は、ポロジェンを含むことを特徴とする請求項1乃至6のいずれか一項に記載の電極合材用液体組成物。
- 請求項1乃至7のいずれか一項に記載の電極合材用液体組成物を、電極基体上に塗布する工程を含むことを特徴とする電極の製造方法。
- 請求項8に記載の電極の製造方法を用いて、電極を製造する工程を含むことを特徴とする電気化学素子の製造方法。
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EP4064382A1 (en) | 2021-03-22 | 2022-09-28 | Ricoh Company, Ltd. | Liquid composition, method for producing electrode, and method for producing electrochemical element |
US11978881B2 (en) | 2019-11-26 | 2024-05-07 | Ricoh Company, Ltd. | Set of liquid compositions and method for manufacturing electrochemical element |
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US11978881B2 (en) | 2019-11-26 | 2024-05-07 | Ricoh Company, Ltd. | Set of liquid compositions and method for manufacturing electrochemical element |
EP4064382A1 (en) | 2021-03-22 | 2022-09-28 | Ricoh Company, Ltd. | Liquid composition, method for producing electrode, and method for producing electrochemical element |
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