JP7387416B2 - 固体電解質、固体電解質膜、電極及びアルカリ金属電池 - Google Patents
固体電解質、固体電解質膜、電極及びアルカリ金属電池 Download PDFInfo
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- JP7387416B2 JP7387416B2 JP2019225342A JP2019225342A JP7387416B2 JP 7387416 B2 JP7387416 B2 JP 7387416B2 JP 2019225342 A JP2019225342 A JP 2019225342A JP 2019225342 A JP2019225342 A JP 2019225342A JP 7387416 B2 JP7387416 B2 JP 7387416B2
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- Prior art keywords
- solid electrolyte
- alkali metal
- meth
- acrylate
- sulfide
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- 239000007784 solid electrolyte Substances 0.000 title claims description 151
- 229910052783 alkali metal Inorganic materials 0.000 title claims description 79
- 239000012528 membrane Substances 0.000 title claims description 68
- 150000001340 alkali metals Chemical class 0.000 title description 20
- -1 alkali metal salt Chemical class 0.000 claims description 111
- 239000000203 mixture Substances 0.000 claims description 85
- 239000003792 electrolyte Substances 0.000 claims description 60
- 239000000178 monomer Substances 0.000 claims description 51
- 239000003795 chemical substances by application Substances 0.000 claims description 32
- 229920000642 polymer Polymers 0.000 claims description 30
- 150000003839 salts Chemical class 0.000 claims description 30
- 229910003480 inorganic solid Inorganic materials 0.000 claims description 11
- 229920000570 polyether Polymers 0.000 claims description 10
- 229910052731 fluorine Inorganic materials 0.000 claims description 9
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 claims description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 7
- 229910001416 lithium ion Inorganic materials 0.000 claims description 7
- 125000004434 sulfur atom Chemical group 0.000 claims description 7
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 229920001187 thermosetting polymer Polymers 0.000 claims description 6
- 229920000058 polyacrylate Polymers 0.000 claims description 5
- 239000011149 active material Substances 0.000 claims description 4
- 150000002825 nitriles Chemical class 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 239000004417 polycarbonate Substances 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 70
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 40
- 238000000034 method Methods 0.000 description 36
- 125000004432 carbon atom Chemical group C* 0.000 description 26
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- 150000001875 compounds Chemical class 0.000 description 20
- 239000003505 polymerization initiator Substances 0.000 description 18
- 239000002994 raw material Substances 0.000 description 17
- 239000002904 solvent Substances 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 125000000217 alkyl group Chemical group 0.000 description 12
- 150000002430 hydrocarbons Chemical group 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 12
- 238000002156 mixing Methods 0.000 description 12
- 239000011230 binding agent Substances 0.000 description 11
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 description 11
- 239000002002 slurry Substances 0.000 description 11
- 125000002947 alkylene group Chemical group 0.000 description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 10
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 9
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 9
- 238000003701 mechanical milling Methods 0.000 description 9
- 239000007773 negative electrode material Substances 0.000 description 9
- 239000007774 positive electrode material Substances 0.000 description 9
- 239000011324 bead Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 description 8
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 7
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
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- 229910001413 alkali metal ion Inorganic materials 0.000 description 6
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- 125000003118 aryl group Chemical group 0.000 description 4
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Images
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- 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
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- Battery Electrode And Active Subsutance (AREA)
Description
[1] 硫黄原子を含む無機固体電解質と、アルカリ金属塩及び塩解離剤を含有する電解質組成物とを含むことを特徴とする固体電解質。
[2] 前記電解質組成物における前記アルカリ金属塩の含有量が50質量%以上であることを特徴とする前記[1]に記載の固体電解質。
[3] 前記電解質組成物がさらに重合体を含むことを特徴とする前記[1]又は[2]に記載の固体電解質。
[4] 前記電解質組成物がさらに光及び/又は熱硬化性単量体を含むことを特徴とする前記[1]又は[2]に記載の固体電解質。
[5] 前記アルカリ金属塩は、下記一般式(1):
MN(SO2R1)(SO2R2) (1)
(式中、Mはアルカリ金属イオンを表す。R1、R2は、同一又は異なって、フッ素原子又は炭素数1~3のフルオロアルキル基を表す。)で表されることを特徴とする前記[1]~[4]のいずれか1つに記載の固体電解質。
[6] 前記塩解離剤が、カーボネート化合物、ニトリル化合物及びスルホニル化合物からなる群より選択される少なくとも1種であることを特徴とする前記[1]~[5]のいずれか1つに記載の固体電解質。
[7] 前記[1]~[6]のいずれか1つに記載の固体電解質を用いて形成されてなる固体電解質膜。
[8] 硫黄原子を含む無機固体電解質と、アルカリ金属塩及び塩解離剤を含有する電解質組成物と、活物質とを含むことを特徴とする電極。
[9] 前記電解質組成物における前記アルカリ金属塩の含有量が50質量%以上であることを特徴とする前記[8]に記載の電極。
[10] 前記電解質組成物がさらに重合体を含むことを特徴とする前記[8]又は[9]に記載の電極。
[11] 前記電解質組成物がさらに光及び/又は熱硬化性単量体を含むことを特徴とする前記[8]又は[9]に記載の電極。
[12] 前記アルカリ金属塩は、下記一般式(1):
MN(SO2R1)(SO2R2) (1)
(式中、Mはアルカリ金属イオンを表す。R1、R2は、同一又は異なって、フッ素原子又は炭素数1~3のフルオロアルキル基を表す。)で表されることを特徴とする前記[8]~[11]のいずれか1つに記載の電極。
[13] 前記塩解離剤が、カーボネート化合物、ニトリル化合物及びスルホニル化合物からなる群より選択される少なくとも1種であることを特徴とする前記[8]~[12]のいずれか1つに記載の電極。
[14] 前記[7]に記載の固体電解質膜及び/又は前記[8]~[12]のいずれか1つに記載の電極を備えるアルカリ金属電池。
本実施形態に係る固体電解質は、硫黄原子を含む無機固体電解質と、アルカリ金属塩及び塩解離剤を含有する電解質組成物とを含む。この固体電解質は、全固体二次電池の電解質膜及び/又は電極に好適に用いられる。
硫黄原子を含む無機固体電解質(以下「硫化物系固体電解質」ともいう)は、硫化リチウムと、周期律表第13~15族の元素を含む硫化物(以下「特定の硫化物」ともいう)とをそれぞれ所定のモル%で含む原料を混合して得られるものである。この硫化物系固体電解質は、ガラス状(非晶質系)のものでもよく、結晶質系の(結晶性を有する)ものでもよいが、イオン伝導性を向上する観点から、非晶質系のものが好ましい。
硫化物系固体電解質の製造方法は、特に制限されず、溶融急冷法、メカニカルミリングによる方法、不活性ガス又は真空中で500℃以下にて焼成する方法、原料混合物の粉砕/ペレット化/焼成を繰り返す方法等が挙げられる。また、これらの製造方法を組み合わせてもよく、メカニカルミリングの後に焼成を行ってもよい。なお、硫化リチウムが酸素や水と反応性を有するため、窒素やアルゴンなどの不活性乾燥ガス雰囲気下や真空中で反応を行うことが好ましい。
電解質組成物は、アルカリ金属塩及び塩解離剤を含有する。
アルカリ金属塩を構成するアルカリ金属としては、リチウム、ナトリウム、カリウム、ルビジウム、セシウム、フランシウム等が挙げられる。これらの中では、リチウム、ナトリウム及びカリウムが好ましく、リチウムがより好ましい。
[化1]
MN(SO2R1)(SO2R2) (1)
で表される化合物がより好ましい。
塩解離剤は、アルカリ金属塩のイオンへの解離を促進するものであれば特に制限されないが、ヘテロ元素を有する化合物が好ましい。ヘテロ元素を有する化合物としては、カーボネート化合物、ニトリル化合物、スルホニル化合物、カルボン酸無水物、硫酸エステル化合物、チオエーテル化合物、亜硫酸エステル化合物、含窒素環状化合物等が挙げられる。これら塩解離剤は、それぞれ単独で用いてもよく、2種類以上を併用してもよい。塩解離剤の中では、アルカリ金属塩のイオンへの解離がより促進され、アルカリ金属カチオンのイオン伝導度及び輸率を向上する観点から、カーボネート化合物、ニトリル化合物及びスルホニル化合物が好ましく、スルホニル化合物及びニトリル化合物がより好ましく、スルホニル化合物がさらに好ましい。
ロニトリル、2,4-ジメチルグルタロニトリル、2,2,3,3-テトラメチルグルタロニトリル、2,2,4,4-テトラメチルグルタロニトリル、2,2,3,4-テトラメチルグルタロニトリル、2,3,3,4-テトラメチルグルタロニトリル、マレオニトリル、フマロニトリル、1,4-ジシアノペンタン、2,6-ジシアノヘプタン、2,7-ジシアノオクタン、2,8-ジシアノノナン、1,6-ジシアノデカン、1,2-ジジアノベンゼン、1,3-ジシアノベンゼン、1,4-ジシアノベンゼン、3,3’-(エチレンジオキシ)ジプロピオニトリル、3,3’-(エチレンジチオ)ジプロピオニトリル及び3,9-ビス(2-シアノエチル)-2,4,8,10-テトラオキサスピロ[5,5]ウンデカン等が挙げられる。
[化2]
NC-R3-CN (2)
(式中、R3は、炭素数1~6のアルキル基又は炭素数6~10のアリール基を表す。)で表される化合物がより好ましい。
電解質組成物は、さらに固体電解質との結着性を付与する観点から、ポリエーテル系重合体、(メタ)アクリル系重合体、ニトリル系重合体、フッ素系重合体、ポリエーテル系重合体及びポリカーボネート重合体からなる群より選択される少なくとも1種の重合体を含んでいてもよい。
電解質組成物は、さらに光及び/又は熱硬化性単量体(以下単に「硬化性単量体」ともいう)を含んでいてもよい。
電解質組成物は、上述の硬化性単量体と共に、さらに重合開始剤を含んでいてもよい。重合開始剤としては、光ラジカル重合開始剤や、熱ラジカル開始剤、アニオン重合開始剤、光アニオン重合開始剤、エポキシ樹脂硬化剤等が挙げられる。これらの重合開始剤は、それぞれ単独で用いてもよく、2種類以上を併用してもよい。
電解質組成物は、例えば、アルカリ金属塩、塩解離剤、必要に応じて、硬化性単量体、重合開始剤、各種添加剤等を混合し、ビーズミル、ボールミル、攪拌型混合機等を用いて分散させることによって調製できる。
本実施形態に係る固体電解質膜は、本実施形態の固体電解質を用いて形成される。即ち、この固体電解質膜は、硫化物系固体電解質及び電解質組成物から構成されるため、当該固体電解質膜を備える電池は、その界面抵抗が低く、且つ経時変化による抵抗の増大が抑制され、安定性に優れる。
本実施形態に係る電極は、硫化物系固体電解質及び電解質組成物と共に、活物質とを含む。この電極は、硫化物系固体電解質及び電解質組成物を含むため、当該電極を備える電池は、その界面抵抗が低く、且つ経時変化による抵抗の増大が抑制され、安定性に優れる。電極は、正極及び負極のいずれに用いてもよい。
正極は、正極集電体及び正極合材層を含み、正極合材層が正極集電体上に形成されている。
負極は、負極集電体及び負極合材層を含み、負極合材層が負極集電体上に形成されている。
電極の製造方法の具体例としては、スラリーを調製し、得られたスラリーを用いて電極を形成する方法等が挙げられる。スラリーの調製方法としては、硫化物系固体電解質と、正極活物質又は負極活物質と、導電助剤と、電解質組成物成分として、アルカリ金属塩、塩解離剤、及び必要に応じて重合体と、結着材とを溶媒で混合し、ビーズミル、ボールミル、攪拌型混合機等を用いて分散させることによって調製する方法;硫化物系固体電解質と、正極活物質又は負極活物質と、予め調整した電解質組成物(換言すると、支持体を含まない固体電解質(B))と、必要に応じて結着材とを溶媒で混合し、ビーズミル、ボールミル、攪拌型混合機等を用いて分散させることによって調製する方法等が挙げられる。
本実施形態に係るアルカリ金属電池は、電極(正極及び負極)と、正極及び負極との間に設けられた固体電解質膜とから構成され、この固体電解質膜が正極及び負極等と共に外装ケースに収容されている。本実施形態では、本実施形態の固体電解質膜及び電極を備える。そのため、このアルカリ金属電池は、その界面抵抗が低く、且つ経時変化による抵抗の増大が抑制され、安定した電池性能を発現できる。なお、当該アルカリ金属電池は、本実施形態の固体電解質膜及び電極のいずれか1つを備えるものでもよいが、界面抵抗の低減と安定化との両立をより一層図る観点から、当該固体電解質膜及び電極を備えるものが好ましい。
(無機固体電解質の作製)
原料として、Li2S(日本化学工業株式会社製、99%)、P2S5(Aldrich社製、98%)を用いて非晶質Li3PS4固体電解質を作製した。具体的には、これらの原料をステンレス(SUS-316)製のポットに、ジルコニアボール(10mmΦ:7個、3mmΦ:10個)とともにアルゴン雰囲気下でO(オー)リングによって密閉し、メカニカルミリング処理を施すことにより、非晶質Li3PS4固体電解質を得た。メカニカルミリング条件は、回転数380rpm、処理時間35時間とした。
前記で得られた非晶質Li3PS4固体電解質を、Φ10mmの加圧治具に67mg投入し、380MPaで1軸加圧することで、厚み0.8mmの電解質ペレット(固体電解質膜(A))を得た。
アルカリ金属塩として1.33gのリチウムビス(フルオロスルホニル)イミド(LiFSI、株式会社日本触媒製)と、塩解離剤として0.27gのジメチルスルホン(富士フイルム和光純薬株式会社製)とをPPバイアル(10mL)に計量し、撹拌混合することで混合物を得た。
前記で得られた電解質溶液を、厚み15μmの銅箔上に塗布した後、200μmのPETフイルムをスペーサーに用いて、上面に厚み50μmのPTFE製のシート(以下単に「PTFEシート」という)を被せ、平行平板プレス機で平坦化させた。超高圧水銀ランプ(4.2mW/cm2(365nm)、50μmのPTFEシート透過後)を用いて、PTFEシートを介して、PTFEシートの両面から各々180秒間UV光を照射して光重合反応を行い、膜厚192μmの固体電解質膜(B)を得た。
固体電解質膜(B)からPTFEシートを剥離した面が固体電解質膜(A)と対向するように、Φ10mmのPTFE製の筒内に、下から順に、Φ9mm銅箔(負極)と、固体電解質膜(A)と、Φ9mmに打ち抜いた固体電解質膜(B)とを重ね合わせた。これにより、固体電解質膜(A)と固体電解質膜(B)とが積層された固体電解質膜(C)を得た。即ち、固体電解質膜(C)は、硫化物系固体電解質と、アルカリ金属塩、塩解離剤、硬化性単量体及び重合開始剤を含有する電解質組成物とを含む固体電解質を用いて形成されてなる固体電解質膜である。この固体電解質(C)を銅箔と共にステンレス製の電極(正極)で挟み、ネジ式の手締めで固定することにより、リチウムイオン二次電池を得た。
前記で得られたリチウムイオン二次電池を40℃の恒温槽に設置した後、ポテンショガルバノスタット(VSP-300、Biologic製)を用いて、周波数1MHz~10mHz、振幅10mVの条件下、2.5時間毎に22.5時間まで、インピーダンスを測定した。
(架橋基含有ポリアルキレンオキシド共重合体の合成)
攪拌機、添加口及び温度センサーを備えた1Lオートクレーブ反応器を窒素により置換後、モレキュラーシーブで脱水処理を施したトルエン286.5部と、t-ブトキシカリウム(1.0Mテトラヒドロフラン溶液)0.85部とを順次投入し、反応器内の圧力がゲージ圧で0.3MPaになるまで窒素で加圧した。
0.2gのリチウムビス(トリフルオロメタンスルホニル)イミド(LiTFSI、LBGグレード、キシダ化学株式会社製)と、0.79gの前記架橋基含有ポリアルキレンオキシド共重合体と、0.01gの重合開始剤(ESACURE KTO46)をPPバイアル(10mL)に計量し、1.6mLのアセトニトリル(LBGグレード、キシダ化学株式会社製)を混合溶解して電解質溶液を得た。
固体電解質膜(B)をポリマー固体電解質膜(D)に変更したこと以外は、実施例1と同様にして、固体電解質膜(A)とポリマー固体電解質膜(D)とが積層された固体電解質膜(E)を形成し、当該固体電解質膜(E)用いてリチウムイオン二次電池を作製し、電池評価を実施した。
実施例1の固体電解質膜(C)及び比較例1の固体電解質膜(E)のバルク抵抗値(膜に対して垂直方向の抵抗値)の増加量(経時変化)を図1に示す。図1の結果から、バルク抵抗値は、比較例1では時間経過に伴って増大したのに対し、実施例1では経時変化がほとんどなく、安定であることが分かった。
Claims (8)
- 硫黄原子を含む無機固体電解質と、アルカリ金属塩及び塩解離剤を含有する電解質組成物とを含む固体電解質であって、
前記アルカリ金属塩としてLiN(FSO 2 ) 2 を含み、
前記塩解離剤として、カーボネート化合物、ニトリル化合物及びスルホニル化合物からなる群より選択される少なくとも1種を含み、
前記電解質組成物に含まれる成分の総量100質量%に対する前記アルカリ金属塩の含有量が50質量%以上であることを特徴とする固体電解質。 - 前記電解質組成物がさらにポリエーテル系重合体、(メタ)アクリル系重合体、ニトリル系重合体、フッ素系重合体、ポリエーテル系重合体及びポリカーボネート重合体からなる群より選択される少なくとも1種の重合体を含むことを特徴とする請求項1に記載の固体電解質。
- 前記電解質組成物がさらに光及び/又は熱硬化性単量体を含むことを特徴とする請求項1又は2に記載の固体電解質。
- 前記電解質組成物1kg当たりの前記アルカリ金属塩の濃度が1.8mol/kg以上であることを特徴とする請求項1~3のいずれか1項に記載の固体電解質。
- 前記電解質組成物に含まれる成分の総量100質量%に対する前記塩解離剤の含有量が5質量%以上であることを特徴とする請求項1~4のいずれか1項に記載の固体電解質。
- 請求項1~5のいずれか1項に記載の固体電解質を用いて形成されてなる固体電解質膜。
- 請求項1~5のいずれか1項に記載の固体電解質と、活物質とを含むことを特徴とする電極。
- 請求項6に記載の固体電解質膜及び/又は請求項7に記載の電極を備えるリチウムイオン二次電池。
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