JP2018515893A - アルカリバッテリーの為のハイブリッド型固体シングルイオン伝導性電解質 - Google Patents
アルカリバッテリーの為のハイブリッド型固体シングルイオン伝導性電解質 Download PDFInfo
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- JP2018515893A JP2018515893A JP2017560533A JP2017560533A JP2018515893A JP 2018515893 A JP2018515893 A JP 2018515893A JP 2017560533 A JP2017560533 A JP 2017560533A JP 2017560533 A JP2017560533 A JP 2017560533A JP 2018515893 A JP2018515893 A JP 2018515893A
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- 150000002500 ions Chemical class 0.000 claims abstract description 22
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- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 3
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- 238000005481 NMR spectroscopy Methods 0.000 description 3
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- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本発明は、米国エネルギー省によって授与された契約番号DE−AC02−05CH11231の下、政府の助成を用いて行った。政府は、本発明において一定の権利を有する。
本出願は、2015年5月21日に出願された米国仮特許出願番号第62/165,079号及び2015年11月12日に出願された米国仮特許出願番号第62/254,486号の利益を主張し、それらの開示内容は、参照によりその全文が本明細書に組み込まれる。
本発明は、リチウムイオンバッテリー、リチウムエアバッテリー及びナトリウムエアバッテリーなどのバッテリーにおいて使用する為のハイブリッド型固体電解質組成物に関する。
各Rは独立に、−OH、−COOH、−COOR’又は−OCOOR’からなる群から選択され、
Rfは、フルオロポリマーセグメントを含み、
各R’は独立に、水素又は脂肪族、芳香族又は混合脂肪族及び芳香族基から選択される]。
本発明において使用する為の適したフルオロポリマーとして、式I、式IIの化合物及びそれらの混合物(例えば、2種以上の異なる両方とも一般式Iの化合物:1種又は複数の一般式Iの化合物及び1種又は複数の一般式IIの化合物、2種以上の異なる一般式IIの化合物を含む)が挙げられる:
各Rは独立に、−OH、−COOH、−COOR’又は−OCOOR’からなる群から選択され、
Rfは、0.2、0.4又は0.5〜5、10又は20Kg/molの重量平均分子量を有するフルオロポリマーセグメント(例えば、パーフルオロポリエーテルセグメントなどのフルオロポリエーテルセグメント)であり、
各R’は独立に、脂肪族、芳香族又は混合脂肪族及び芳香族基(例えば、各々独立に、Rf、ポリエチレングリコール(PEG)などのポリエーテル、PEG炭酸などのポリエーテル炭酸等と関連して与えられるようなフルオロポリマーを含む、アルキル、アルケニル、アルキニル、シクロアルキルアルキル、シクロアルキルアルケニル、シクロアルキルアルキニル、アリールアルキル、アリールアルケニル、アリールアルキニル、ヘテロシクロアルキル、ヘテロシクロアルケニル、ヘテロシクロアルキニルなどからなる群から選択される)から選択される]。
固体であり、アルカリイオン(例えば、リチウム又はナトリウムイオン)を伝導する任意の無機電解質が、本明細書において記載される電解質組成物において使用され得る。これらの無機電解質は、通常、粒子の形態である。無機電解質は、特定の実施形態では、ガラス、ガラス−セラミック又はセラミック粒子であり得る。
種々の実施形態によれば、本明細書に記載される電解質組成物は、無機電解質及びフルオロポリマーを含む固体電解質組成物である。固体電解質組成物は、無機相及び有機ポリマー相を含むハイブリッド又は複合組成物として特性決定され得る。上記のように、無機相は、通常、イオン伝導性粒子の形態である。ポリマー相は、上記のようなイオン伝導性フルオロポリマーであり得る。いくつかの実施形態では、イオン伝導性粒子は、フルオロポリマーマトリックス中に分散される。いくつかの実施形態では、無機電解質は、フルオロポリマーと結合される。いくつかの実施形態では、無機電解質は、フルオロポリマーと結合されない。結合される場合には、結合は、共有結合、イオン結合、ファンデルワールス結合又は水素結合のうち任意の1つ又は複数であり得る。
電解質中のイオンの輸率は、イオンについて電解質中で流れる総電流の割合である。シングルイオン伝導体は、1に近い輸率を有する。本明細書において記載される固体電解質複合体は、シングルイオン伝導体であり、1に近い輸率を有する。
本発明のアルカリ金属バッテリー(アルカリ金属イオンバッテリーと呼ばれることもあり、アルカリ金属−エアバッテリーを含む)は、一般に、(a)アノード、(b)カソード、(c)アノード及びカソードと作動可能に関連している上記のようなハイブリッド固体電解質組成物及び(d)任意選択で、アノード及びカソードを物理的に分離するセパレータを含む(例えば、参照により本明細書に組み込まれる、M.アーマンド(Armand)及びJ.−M.タラスコン(Tarascon)、ビルディング バッテリー バッテリーズ(Building Bettery Batteries)ネイチャー(Nature)第451巻、p.652−657(2008年)を参照のこと)。適したバッテリー成分の例として、それだけには限らないが、参照により本明細書に組み込まれる、米国特許第5,721,070号;同6,413,676号、同7,729,949号及び同7,732,100号に、並びに米国特許出願公開第2009/0023038号、同2011/0311881号及び同2012/0082930号並びにS.−W.キム(Kim)等、アドバンスド エネルギー マテリアルズ(Adv. Energy Mater.)第2巻、p.710−721(2012年)に記載されたものが挙げられる。
試薬等級Li2S(99.9%)及びP2S5(99%)は、Aldrichから購入した。上記で示されるようなヒドロキシ末端パーフルオロポリエーテル(PFPE−ジオール、Mw=1000g/mol)は、Solvayから購入し、リチウムビス(トリフルオロメタンスルホン)イミド(LiTFSI)は、Novolyteから購入した。すべての化学物質は、受け取ったまま使用した。
CDCl3又は重水素化THF−d8中、Bruker Advance 400及び600スペクトロメーターで、19F及び31P−NMRスペクトルを得た。硫化物ガラスペレット及びハイブリッド膜の形態学的特性決定は、エネルギー分散型X線分光法(SEM/EDS)を用い走査型電子顕微鏡によって達成した。すべてのサンプルは、アルゴン下で調製し、測定した。SEM実験は、SEM測定の為に5kV及びEDS測定の為に10kV加速電圧を用い、JEOL−7500F電界放射顕微鏡で実施した。線形レオロジー測定の為に、直径8mm及び厚み1.5mmのハイブリッドペレットを、伝導率測定の為のハイブリッドペレットと同一方法を使用して調製した。レオロジー測定は、Rheometric Scientific ARES Rheostatにおいて実施した。レオメータプラテンを清潔にし、窒素下で30℃に加熱した。プラテンギャップ位置をゼロとし、次いで、サンプルをプラテンの間に入れた。次いで、プラテンを30℃に加熱し、サンプルを1時間平衡にした。各測定温度で、10rad/sの周波数で、動的ひずみ試験を実施して、線形領域における測定を確実にした。次いで、動的周波数試験を線形領域において低ひずみで実施した。
電解質として無機硫化物ガラス又はハイブリッドを使用して、グローブボックス中でアルミニウム対称電池を組み立てた。ガラス及びハイブリッドペレットは、空冷で得た(それぞれ、57MPa及び23MPa)。ボールミリング後、2つの鏡面研磨アルミニウム電極間のペレット型中にガラス粉末を入れた。ペレットの直径及び厚みは、それぞれ、13mm及び約1mmであった。各電極上にアルミニウム集電タブを置く。手動のプレス機を使用してハイブリッド電解質膜(厚さ約250μm)を得た。電極及び電解質間の良好な接触を確実にする為に、ボールミルから得たハイブリッド電解質粉末を、3.17mmの直径の中心穴を有するプレス機の絶縁スペーサー並びに2つの鏡面研磨アルミニウム電極の中心に入れた。プレス機を90℃に5秒間加熱した。アルミニウム集電タブを各電極の上に置く。最後に、ペレット及びハイブリッド膜の両方を、ポーチバッグ中に真空密閉して空気から隔離した。周波数範囲1MHz〜1Hzにおいて50mVのac振幅を用いVMP3(Bio−Logic)を使用して、インピーダンス分光法測定を実施した。インピーダンススペクトルは、温度、T、27℃及び120℃の範囲において、加熱及び冷却スキャンの間10℃間隔で記録した。ガラス電解質又はハイブリッド電解質中の伝導相のイオン伝導率、σは、測定されたサンプル厚、l、スペーサーの断面積S及び電解質抵抗Relから算出される。σ(T)は、以下によって与えられる:
輸率測定の為に、2つのリチウム金属チップ(250μm)間でのハイブリッド膜電解質の手動圧縮によってリチウム対称電池を調製した。各リチウム金属電極上にニッケル集電タブを置き、電池をポーチバッグ中に真空密閉した。定常状態技術を使用して、30℃の温度でのリチウム輸率、t+を推定した(ウォン(Wong)DH等(2014年)リチウムバッテリーの為の不燃性パーフルオロポリエーテルベースの電解質(Nonflammable perfluoropolyether-based electrolytes for lithium batteries)米国科学アカデミー紀要(Proc Natl Acad Sci USA)第111巻(9号):p.3327−333l)。この方法は、直流分極及び交流インピーダンス分光法を組み合わせる。最初の交流インピーダンス測定は、初期界面抵抗、
ハイブリッド膜の電気化学安定性を、図10に示されるようにサイクリックボルタンメトリーによって調べた。測定は、1mV/sのスキャン速度で−0.5から5.0V(Li+/Liに対して)の間の電位範囲で30℃で実施した。低電位電流は、Li+/Li0対の還元及び酸化に対応し、リチウムイオンは、負電位でLi金属に還元され、次いで、0.3Vでのその後の酸化の際にリチウム金属電極からはがし取られる(シーラ(Sylla),S.;サンチェス(Sanchez),J.−Y.;アーマンド(Armand),M.エレクトロケミカ アクタ(Electrochimica Acta)1992年、第37巻、p.1699)。1.5から5V電位範囲にわたって、電流密度は、低いままであり、ハイブリッド電解質が5Vまで安定であることを示す。したがって、ハイブリッド電解質は、リチウムニッケルマンガンコバルト酸化物(NMC)などの高い可能性のある活性材料を含むリチウムバッテリーにおいて使用するのに適していると予測される。
これらのハイブリッド固体電解質の1つの可能性ある適用として、リチウムポリスルフィド溶解の問題に悩まされていることが知られているリチウム硫黄(Li−S)バッテリー用がある。Li−S充電/放電反応プロセスの間に形成されるリチウムポリスルフィド反応中間体(Li2Sx、2≦x≦8)は、多数のバッテリー電解質に高度に可溶性である。したがって、ポリスルフィドは、その形成後に、カソードから及び電解質セパレータ中に拡散し、容量を減衰させ、リチウムアノードでの分解反応につながり得る。固体、無機電解質は、それらが、リチウムイオンの通過を可能にしながらポリスルフィド溶解を防ぐので、この問題を解決する為のますます一般的なアプローチになった(リン(Lin),Z.;リュー(Liu),Z.;フー(Fu),W.;ダドニー(Dudney),NJ;リャン(Liang),C.アンゲワンテ ケミー インターナショナル エディション(Angew Chem Int Ed)2013年、第52巻(29号):p.7460−7463)。
Claims (29)
- 固体電解質組成物であって、
無機固体電解質及びイオン伝導性フルオロポリマーを含む複合体を含み、ここで、無機固体電解質及びイオン伝導性フルオロポリマーの各々のカチオン輸率は、少なくとも0.9である、固体電解質組成物。 - カチオン輸率が、リチウム輸率である、請求項1に記載の組成物。
- アルカリ金属塩をさらに含む、請求項1に記載の組成物。
- 前記アルカリ金属塩が、リチウム塩を含む、請求項3に記載の組成物。
- 前記アルカリ金属塩が、ナトリウム塩を含む、請求項3に記載の組成物。
- 前記複合体が、90〜99.5重量%の量で前記組成物中に含まれ、
前記アルカリ金属塩が、0.5〜10重量%の量で前記組成物に含まれる、
請求項3から5に記載の組成物。 - Rfが、パーフルオロポリエーテルセグメントを含む、請求項7に記載の組成物。
- 各Rが、−OH及び−COOHからなる群から選択される、請求項7又は8に記載の組成物。
- 前記フルオロポリマーが、式Iの化合物を含む、請求項7から9に記載の組成物。
- 前記フルオロポリマーは、式IIの化合物を含む、請求項7から9に記載の組成物。
- 前記無機固体電解質が、アルカリイオンを伝導し、ペロブスカイト、ガーネット、チオ−LISICON、NASICON、ガラスセラミック、ナトリウムスーパーイオン伝導体、酸化物ガラス又は硫化物ガラスを含む、請求項1から11に記載の組成物。
- ペロブスカイトが、Li3xLa(2/3)−xTiO3を含み、
ガーネットが、Li7La3Zr2O12を含み、
チオ−LISICONが、Li10SnP2S12を含み、
NASICONが、Li1.3Al0.3Ti1.7(PO4)3を含み、
ナトリウムスーパーイオン伝導体が、Na1+xZr2SixP3−xO12又は50Na2S−50P2S5を含み、
酸化物ガラスが、Li3BO3−Li2SO4、Li2O−P2O5又はLi2O−SiO2を含み、
硫化物ガラスが、Li2S−SiS2又はLiI−Li2S−B2S3を含む、
請求項12に記載の組成物。 - 前記無機固体電解質が、75Li2S・25P2S5を含む硫化物ガラスを含む、請求項1から11に記載の組成物。
- 前記アルカリ金属塩が、リチウムビス(トリフルオロメタン−スルホン)イミド(LiTFSI)を含む、請求項3及び6から14に記載の組成物。
- 前記フルオロポリマー及びアルカリ金属塩が一緒に、組成物中に約23重量%の量で含まれる、請求項7から15に記載の組成物。
- 前記組成物が、室温で少なくとも約10−4S/cmのイオン伝導率を有する、請求項1から16に記載の組成物。
- 室温でLi+/Liに対して最大5Vの安定電位窓を有する、請求項1から17に記載の組成物。
- 電極分解防止剤をさらに含む、請求項1から18に記載の組成物。
- 揮発性炭酸溶媒を実質的に含まない、請求項1から19に記載の組成物。
- −120℃から−20℃の間のガラス転移温度Tgを有する、請求項1から20に記載の組成物。
- Kohler開放式迅速引火試験装置において、235℃の温度に加熱され、次いで、炎に15秒間接触された場合に点火しない、請求項1から21に記載の組成物。
- 前記フルオロポリマーが、アモルファスである、請求項1から22に記載の組成物。
- 柔軟性固体である、請求項1から23に記載の組成物。
- フィルムの形態である、請求項1から24に記載の組成物。
- フルオロポリマーが、ポリスルフィドを溶媒和しない、請求項1から25のいずれかに記載の組成物。
- 固体電解質組成物であって、
(a)フルオロポリマーと結合している無機固体電解質を含む複合体と、
(b)任意選択で、アルカリ金属塩と
を含む、固体電解質組成物。 - バッテリーであって、
(a)アノードと、
(b)カソードと、
(c)前記アノード及びカソードと作動可能に関連している固体電解質組成物と
を含み、
前記電解質組成物が、請求項1から27に記載の組成物を含む、バッテリー。 - 前記カソードが、硫黄カソードを含む、請求項28に記載のバッテリー。
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US201562254486P | 2015-11-12 | 2015-11-12 | |
US62/254,486 | 2015-11-12 | ||
PCT/US2016/033315 WO2016187448A1 (en) | 2015-05-21 | 2016-05-19 | Hybrid solid single-ion-conducting electrolytes for alkali batteries |
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