JP2019102188A - 非水電解質、非水電解質蓄電素子及び非水電解質蓄電素子の製造方法 - Google Patents
非水電解質、非水電解質蓄電素子及び非水電解質蓄電素子の製造方法 Download PDFInfo
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- JP2019102188A JP2019102188A JP2017229587A JP2017229587A JP2019102188A JP 2019102188 A JP2019102188 A JP 2019102188A JP 2017229587 A JP2017229587 A JP 2017229587A JP 2017229587 A JP2017229587 A JP 2017229587A JP 2019102188 A JP2019102188 A JP 2019102188A
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Images
Classifications
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
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- C07D239/26—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to ring carbon atoms
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Abstract
Description
式(2)中、R5〜R7は、それぞれ独立して、水素原子、又は−NRb 2、−ORb若しくは−SRbで表される基である。Rbは、それぞれ独立して、水素原子又は炭素数1〜6のアルキル基である。但し、R5〜R7のうちの少なくとも1つは、それぞれ独立して、−SRbで表される基である。)
式(2)中、R5〜R7は、それぞれ独立して、水素原子、又は−NRb 2、−ORb若しくは−SRbで表される基である。Rbは、それぞれ独立して、水素原子又は炭素数1〜6のアルキル基である。但し、R5〜R7のうちの少なくとも1つは、それぞれ独立して、−SRbで表される基である。
当該非水電解質は、非水溶媒、電解質塩、及び添加剤を含有する。当該非水電解質は、蓄電素子に用いられる。なお、当該非水電解質は、液体に限定されるものではない。すなわち、当該非水電解質は、液体状のものだけに限定されず、固体状やゲル状のもの等も含まれる。
上記非水溶媒としては、一般的な蓄電素子用非水電解質の非水溶媒として通常用いられる公知の非水溶媒を用いることができる。上記非水溶媒としては、環状カーボネート、鎖状カーボネート、エステル、エーテル、アミド、スルホン、ラクトン、ニトリル等を挙げることができる。これらの中でも、環状カーボネート又は鎖状カーボネートを少なくとも用いることが好ましく、環状カーボネートと鎖状カーボネートとを併用することがより好ましい。環状カーボネートと鎖状カーボネートとを併用する場合、環状カーボネートと鎖状カーボネートとの体積比(環状カーボネート:鎖状カーボネート)としては、特に限定されないが、例えば5:95以上50:50以下とすることが好ましい。
上記電解質塩としては、一般的な蓄電素子用非水電解質の電解質塩として通常用いられる公知の電解質塩を用いることができる。上記電解質塩としては、リチウム塩、ナトリウム塩、カリウム塩、マグネシウム塩、オニウム塩等を挙げることができるが、リチウム塩が好ましい。
上記添加剤は、下記式(1)又は式(2)で表される化合物である。当該非水電解質は、上記添加剤を含有するため、非水電解質蓄電素子の直流抵抗を低くし、かつ充放電サイクル後の容量維持率を高めることができる。また、当該非水電解質は、非水電解質蓄電素子の充放電サイクル後の直流抵抗やクーロン効率の維持率を高めることもできる。
式(1)中、R1〜R4は、それぞれ独立して、水素原子、又は−NRa 2、−ORa、−SRa、−COORa、−CORa、−SO2Ra若しくは−SO3Raで表される基である。Raは、それぞれ独立して、水素原子又は炭化水素基である。但し、R1〜R4のうちの少なくとも1つは、−ORa、−SRa、−COORa、−CORa、−SO2Ra又は−SO3Raで表される基である。
式(2)中、R5〜R7は、それぞれ独立して、水素原子、又は−NRb 2、−ORb若しくは−SRbで表される基である。Rbは、それぞれ独立して、水素原子又は炭素数1〜6のアルキル基である。但し、R5〜R7のうちの少なくとも1つは、それぞれ独立して、−SRbで表される基である。
当該非水電解質は、上記非水溶媒、上記電解質塩、及び上記添加剤以外の他の成分をさらに含有していてもよい。上記他の成分としては、1,3−プロペンスルトン(PRS)、ビニルエチレンカーボネート(VEC)、ビニレンカーボネート(VC)、アジポニトリル(AN)、ジグリコールサルフェート(DGLST)、ペンチルグリコールサルフェート(PEGLST)、硫酸プロピレン(PGLST)、リチウムビス(トリフルオロメチルスルフォニル)アミド(LiTFSA)、リチウムテトラフルオロオキサレートホスフェート(LiFOP)等を挙げることができ、これらの中でも、PRS、VC及びANが好ましい。これらの成分は、負極上に良好な被膜を形成し、本発明の効果をより高めることができる。また、これらの成分と上記添加剤とを併用することで、初期の放電容量及び直流抵抗、並びに充放電サイクル後の直流抵抗の維持率などを改善することができる。なお、当該非水電解質における上記他の成分の含有量の下限としては、0.01質量%が好ましく、0.1質量%がより好ましく、0.5質量%がさらに好ましい。一方、この含有量の上限としては、5質量%が好ましく、2質量%がより好ましい。
本発明の一実施形態に係る非水電解質蓄電素子は、正極、負極及び非水電解質を有する。以下、非水電解質蓄電素子の一例として、非水電解質二次電池(以下、単に「二次電池」ともいう。)について説明する。上記正極及び負極は、通常、セパレータを介して積層又は巻回により交互に重畳された電極体を形成する。この電極体はケースに収納され、このケース内に非水電解質が充填される。上記非水電解質として、本発明の一実施形態に係る上述した非水電解質が用いられる。当該非水電解質は、正極と負極との間に介在する。上記ケースとしては、二次電池のケースとして通常用いられる公知の金属ケース、樹脂ケース等を用いることができる。以下、当該非水電解質以外の当該二次電池の構成要素について説明する。
上記正極は、正極基材、及びこの正極基材に直接又は中間層を介して配される正極活物質層を有する。
上記負極は、負極基材、及びこの負極基材に直接又は中間層を介して配される負極活物質層を有する。上記中間層は正極の中間層と同様の構成とすることができる。
上記セパレータの材質としては、例えば織布、不織布、多孔質樹脂フィルム等が用いられる。これらの中でも、強度の観点から多孔質樹脂フィルムが好ましく、非水電解質の保液性の観点から不織布が好ましい。上記セパレータの主成分としては、強度の観点から例えばポリエチレン、ポリプロピレン等のポリオレフィンが好ましく、耐酸化分解性の観点から例えばポリイミドやアラミド等が好ましい。また、これらの樹脂を複合してもよい。
本発明の一実施形態に係る非水電解質蓄電素子の製造方法は、当該非水電解質を用いる非水電解質蓄電素子の製造方法である。当該製造方法は、上述した式(1)又は式(2)で表される添加剤を含有する非水電解質を用いること以外は、特に限定されない。上述した二次電池の場合、例えば、正極を作製する工程、負極を作製する工程、非水電解質を調製する工程、正極及び負極をセパレータを介して積層又は巻回することにより交互に重畳された電極体を形成する工程、正極及び負極(電極体)を容器に収容する工程、並びに上記容器に上記非水電解質を注入する工程を備える。注入後、注入口を封止することにより製造することができる。
本発明は上記実施形態に限定されるものではなく、上記態様の他、種々の変更、改良を施した態様で実施することができる。例えば、正極及び負極において、中間層を設けなくてもよく、明確な層構造を有していなくてもよい。例えば正極及び負極は、メッシュ状の基材に活物質が担持された構造などであってもよい。また、上記実施の形態においては、非水電解質蓄電素子が二次電池である形態を中心に説明したが、その他の非水電解質蓄電素子であってもよい。その他の非水電解質蓄電素子としては、キャパシタ(電気二重層キャパシタ、リチウムイオンキャパシタ)等が挙げられる。
・MPC :下記式(1a)で表される化合物
・DMSP:下記式(1b)で表される化合物
・MCP :下記式(1c)で表される化合物
・PMD :下記式(1x)で表される化合物
・DTD:下記式(2b)で表される化合物
・TAZ:下記式(2x)で表される化合物
・TAC:下記式(2y)で表される化合物
・VC :ビニレンカーボネート
・AN :アジポニトリル
(非水電解質の調製)
FECとDMCとEMCとを10:40:50の体積比で混合した非水溶媒に、電解質塩としてLiPF6を1.2mol/Lの濃度で溶解させ、これに添加剤としてMPCを2.0質量%添加し、実施例1の非水電解質を得た。
上記非水電解質を用い、以下の手順にて、実施例1の非水電解質蓄電素子(二次電池)を得た。
(正極の作製)
正極活物質として、LiNi0.8Co0.15Al0.05O2、アセチレンブラック及びポリフッ化ビニリデンを91:4.5:4.5の質量比で含有し、N−メチル−2−ピロリドンを溶剤(分散媒)とする正極ペーストを調整した。この正極ペーストをアルミニウム箔の表面に塗布し、ローラープレス機により加圧成形して正極活物質層を形成した。その後、100℃で12時間減圧乾燥することにより、正極を得た。
(負極の作製)
負極活物質として、グラファイト、スチレンブタジエンゴム及びカルボキシメチルセルロースを95:2:3の質量比で含有し、水を溶剤(分散媒)とする負極ペーストを調整した。この負極ペーストを銅箔の表面に塗布し、ローラープレス機により加圧成形して負極活物質層を形成した。その後、100℃で12時間減圧乾燥することにより、負極を得た。
(組み立て)
上述の正極と負極とをポリオレフィン製多孔質樹脂フィルムセパレータを介して巻回することで電極体を作成した。この電極体をアルミケースに挿入した後に、ケースの蓋をレーザ溶接した。ケースに設けられた注液孔を介して、ケースに上述の非水電解質を注入したあと、注液孔を封止し、非水電解質二次電池を得た。
添加剤として、表1〜3に記載の種類及び量の添加剤を添加したこと以外は実施例1と同様にして、実施例2〜7及び比較例1〜5の非水電解質及び非水電解質蓄電素子を得た。
(初期の性能評価)
各非水電解質蓄電素子に対し、容量確認試験として、25℃で4.35Vまで0.33Cの定電流充電したのちに、4.35Vで定電圧充電した。充電の終了条件は、総充電時間が5時間となるまでとした。充電後に10分間の休止期間を設けたのちに、25℃で2.50Vまで1.0Cで定電流放電した。これにより、初期の放電容量を求めた。また、50%SOC、25℃又は−10℃における直流抵抗(DCR)を測定した。表1の各実施例及び比較例については、各非水電解質蓄電素子の厚さを測定した。表2の実施例4及び比較例2については、上記容量確認試験における放電容量を充電電気量で除することによってクーロン効率(%)を求めた。測定結果の一部を表1〜3に示す。
各非水電解質蓄電素子に対し、以下のサイクル試験を行った。45℃において、充電電流0.33C、充電終止電圧4.35Vとして定電流定電圧充電した。充電の終了条件は、総充電時間が5時間となるまでとした。その後、10分間の休止期間を設けた。その後、放電電流1.0C、放電終止電圧2.50Vとして定電流放電を行い、その後、10分間の休止期間を設けた。いずれの実施例及び比較例も、この充放電を500サイクル実施した。
表1、2の各実施例及び比較例については、サイクル試験後、上記「初期の性能評価」と同様の方法にて容量確認試験を行った。充放電サイクル試験後の容量を初期の容量で除し、容量の充放電サイクル後維持率(容量維持率)を求めた。
表1の各実施例及び比較例については、サイクル試験後、各非水電解質蓄電素子の厚さを測定し、充放電サイクル試験後の厚さを初期の厚さで除し、厚さの充放電サイクル後維持率を求めた。
表1の各実施例及び比較例については、サイクル試験後、上記「初期の性能評価」と同様の方法にて、50%SOC、25℃における直流抵抗(DCR)を測定した。充放電サイクル試験後のDCRを初期のDCRで除し、DCRの充放電サイクル後維持率を求めた。
表2の実施例4及び比較例2については、サイクル試験後の容量確認試験において、充電電気量及び放電容量を測定し、放電容量を充電電気量で除することによってクーロン効率(%)を求めた。充放電サイクル試験後のクーロン効率を初期のクーロン効率で除し、クーロン効率の充放電サイクル後維持率を求めた。
表3の各実施例及び比較例については、サイクル試験後、上記「初期の性能評価」と同様の方法にて容量確認試験、及び50%SOC、25℃又は−10℃におけるにおける直流抵抗(DCR)を測定した。
それぞれの測定結果を、比較とする比較例の値を基準とした相対値として表1〜3に示す。なお、表中の「−」は、測定を行っていないことを示す。
2 電極体
3 容器
4 正極端子
4’ 正極リード
5 負極端子
5’ 負極リード
20 蓄電ユニット
30 蓄電装置
Claims (6)
- 下記式(1)又は式(2)で表される添加剤を含有する蓄電素子用の非水電解質。
式(2)中、R5〜R7は、それぞれ独立して、水素原子、又は−NRb 2、−ORb若しくは−SRbで表される基である。Rbは、それぞれ独立して、水素原子又は炭素数1〜6のアルキル基である。但し、R5〜R7のうちの少なくとも1つは、それぞれ独立して、−SRbで表される基である。) - 上記添加剤が上記式(1)で表され、
上記R1〜R4が、それぞれ独立して、水素原子、又は−ORa、−SRa、−COORa、−CORa、−SO2Ra若しくは−SO3Raで表される基である請求項1の非水電解質。 - 上記添加剤が上記式(1)で表され、
上記R1〜R4のうちの少なくとも1つが、−SRa、−SO2Ra又は−SO3Raで表される基である請求項1又は請求項2の非水電解質。 - 上記添加剤が上記式(2)で表され、
上記R5〜R7が、それぞれ独立して、−ORb又は−SRbで表される基である請求項1の非水電解質。 - 請求項1から請求項4のいずれか1項の非水電解質を有する非水電解質蓄電素子。
- 請求項1から請求項4のいずれか1項の非水電解質を用いる非水電解質蓄電素子の製造方法。
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JP7504740B2 (ja) | 2020-09-25 | 2024-06-24 | Muアイオニックソリューションズ株式会社 | 非水電解液用添加剤、非水電解液、蓄電デバイスおよびトリアジン化合物 |
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