JP2016519412A - 電池用の固体カソライト又は電解質 - Google Patents
電池用の固体カソライト又は電解質 Download PDFInfo
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- JP2016519412A JP2016519412A JP2016514103A JP2016514103A JP2016519412A JP 2016519412 A JP2016519412 A JP 2016519412A JP 2016514103 A JP2016514103 A JP 2016514103A JP 2016514103 A JP2016514103 A JP 2016514103A JP 2016519412 A JP2016519412 A JP 2016519412A
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- catholyte
- positive electrode
- lithium
- sulfur
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- Granted
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- 239000003792 electrolyte Substances 0.000 title description 14
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- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 106
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 105
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 99
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 98
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
- C04B35/6262—Milling of calcined, sintered clinker or ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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Abstract
Description
本出願は、様々な目的のために共に内容全体の引用により全容が本明細書中に組み込まれている、2013年5月15日出願の米国仮特許出願第61/823,407号及び2014年2月5日出願の同第61/935,956号の優先権を主張するものである。
一部の例では、本発明の一実施態様は、一般に、所望のイオン伝導率を有する固体カソライト又は電解質材料に関する。より詳細には、本発明の一実施態様は、活物質の高い質量負荷、迅速な充電/放電、及び広範な動作温度を可能にするために正極の全イオン伝導率を改善するカソライト材料のための方法及び構造を提供する。単なる例として、本発明は、固体電池セルに適用されるが、他の適用もあり得る。
本発明の一実施態様によると、所望のイオン伝導率を有する固体カソライト又は電解質材料に関連した技術が提供される。より詳細には、本発明の一実施態様は、活物質の高い質量負荷、迅速な充電/放電、及び広範な動作温度を可能にするために正極の全イオン伝導率を改善するカソライト材料のための方法及び構造が提供される。単なる例として、本発明は、固体電池セルに適用されるが、他の適用も可能である。
本発明の一実施態様によると、所望のイオン伝導率を有する固体カソライト又は電解質材料に関連した技術が提供される。より詳細には、本発明の一実施態様は、活物質の高い質量負荷、迅速な充電/放電、及び広範な動作温度を可能にするために正極の全イオン伝導率を改善するカソライト材料のための方法及び構造を提供する。単なる例として、本発明は、固体電池セルに適用されるが、他の適用も可能である。
15:2:1
5:1:1
5:1:1
5:1:1
1.基板部材を用意する;
2.充電及び放電期間中に主活性領域が第1の体積から第2の体積に膨張又は収縮するように、正極領域内に空間的に配置された複数の第1の活性領域を含む該主活性領域を形成する;
3.正極領域の空間領域内に空間的に閉じ込められ、かつ第1の活性領域によって占められていない空間領域内に空間的に配置されたカソライト材料を形成する。一例では、カソライト材料は、多結晶状態に構成された、リチウム、金属、リン、及び硫黄(「LMPSO」)含有材料を含む;
4.任意に、カソライト材料内に硫黄種を実質的に維持するように正極材料の露出領域を覆うように形成される保護材料を形成する;
5.正極活物質、電子伝導性添加剤、バインダー、及び他の要素を形成する;
6.正極成分を溶媒と一緒に混合してスラリーにして、該スラリーを前記基板に堆積させ;該基板を乾燥させる;
7.固体電池装置を完成させる;
8.電池装置を梱包する;及び
9.電池装置を輸送する。
一例では、本発明は、正極領域を含むエネルギー保存装置を提供し、該正極領域は、該正極領域内に空間的に配置された複数の第1の活性領域を含む主活性領域であって、充電及び放電期間中に第1の体積から第2の体積に膨張又は収縮する、該主活性領域;該正極領域の空間領域内に空間的に閉じ込められ、かつ該第1の活性領域によって占められていない空間領域内に空間的に配置されたカソライト材料であって、多結晶状態に構成された、リチウム、ゲルマニウム、リン、及び硫黄(「LGPS」)含有材料を含む、該カソライト材料;LGPS含有材料内に含められた酸素種であって、LGPSO材料を形成するために硫黄種に対して1:2以下の比率を有する、該酸素種;及び該カソライト材料内に硫黄種を実質的に維持するために正極材料の露出領域を覆うように形成された保護材料を含む。特定の実施態様では、酸素種は、LGPSO材料の20%未満である。一部の実施態様では、硫黄含有種は、LGPSO材料の約20〜60%である。他の実施態様では、閉じ込め材料は、障壁材料として構成される。他の実施態様では、閉じ込め材料は、硫黄含有種の主活性領域内の要素との相互作用を実質的に防止する。なお他の実施態様では、主活性領域は、正極領域の約50%を超え;かつカソライト材料は、正極領域の約30%未満である。他の実施態様では、閉じ込め材料は、リチウム種が該閉じ込め材料中を移動するのを選択的に可能にするように構成され、該閉じ込め材料は、該リチウム種が該閉じ込め材料中を移動するのを可能にする複数の空間的開口部を備える。なお他の実施態様では、カソライト材料は、主活性領域を含む正極領域を実質的に満たして、該正極領域を画定する実質的に均一な厚さの材料を形成するように構成されている。
Buschmannらの文献「リチウム金属電極動力学及び固体リチウムイオン導体「Li7La3Zr2O12」及びLi7-xLa3Zr2-xTaxO12のイオン伝導率(Lithium metal electrode kinetics and ionic conductivity of the solid lithium ion conductors “Li7La3Zr2O12” and Li7-xLa3Zr2-xTaxO12)」(J. Power Sources 206 (2012) 236-244)、DOI: 10.1016/j.jpowsour.2012.01.094;及び
Ohtaらの文献「ガーネット型酸化物Li7-xLa3(Zr2-x、Nbx)O12(x=0〜2)における高いリチウムイオン伝導(High lithium ionic conductivity in the garnet-type oxide Li7-xLa3(Zr2-x,Nbx)O12 (x=0-2))」(J. Power Sources 196 (2011) 3342-3345)、DOI: 10.1016/j.jpowsour.2010.11.089。
表 A. XPS分析に基づいた組成
表B. 7Li及び31PのNMR分析に基づいた化学環境
Claims (66)
- 正極領域を含むエネルギー保存装置であって、該正極領域が:
充電及び放電期間中に第1の体積から第2の体積に膨張又は収縮する活物質領域;
該活性領域によって占められていない空間領域内に空間的に閉じ込められたカソライト材料であって、それぞれ多結晶状態又は非晶質状態のいずれかに形成された、リチウム、ゲルマニウム、リン、及び硫黄(「LGPS」)材料、又はリチウム、シリコン、リン、及び硫黄(「LSPS」)材料のいずれかを含む、該カソライト材料;
該LGPS又はLSPS材料内の酸素種であって、LGPSO又はLSPSO材料を形成するために硫黄種に対して1:2以下の比率を有する、該酸素種;及び、任意に、
該カソライト材料内の該硫黄種を実質的に維持するために該活物質の露出領域を覆う保護材料、を含む、前記装置。 - 前記酸素種が、前記LGPSO又はLSPSO材料の20 at%未満である、請求項1記載の装置。
- 前記酸素種が、前記硫黄種に対して約0の比率を有する、請求項1記載の装置。
- 前記酸素種が、前記硫黄種に対して0の比率を有する、請求項1記載の装置。
- 硫黄含有種が、前記LGPSO又はLSPSO材料の約20〜60 vol%である、請求項1記載の装置。
- 前記保護材料が、硫黄含有種の前記活性領域内の要素との相互作用を実質的に防止する、請求項1記載の装置。
- 前記活性領域が、前記正極領域の約50%を超え;かつ前記カソライト材料が、該正極領域の約30%未満である、請求項1記載の装置。
- 前記活性領域が、前記正極領域の約45%を超え;かつ前記カソライト材料が、該正極領域の約30%未満である、請求項1記載の装置。
- 前記カソライト材料の近傍内に形成されたポリマー材料を更に含む、請求項1記載の装置。
- 前記ポリマー材料がリチウム種を含む、請求項9記載の装置。
- 前記ポリマー材料が、前記カソライト材料を覆っている、請求項9記載の装置。
- 前記カソライト材料が複数の粒子を含む、請求項1記載の装置。
- 前記活性領域が、約20 nm〜約10μmのメディアン径を有するクラスターを含む、請求項1記載の装置。
- 前記カソライト材料が、約10 nm〜約300 nmのメディアン径を有するクラスターを含む、請求項1記載の装置。
- 前記カソライトのクラスターのメディアン径が80 nmよりも小さい、請求項14記載の装置。
- 前記カソライト材料が、前記正極活性領域の周りに複数のシェル構造を含む、請求項1記載の装置。
- 前記カソライト材料が、約20 nm〜約300 nmのメディアン径を有する複数の粒子を含む、請求項1記載の装置。
- 前記粒子の80%が、約20 nm〜約300 nmのメディアン径を有する、請求項17記載の装置。
- 複数の前記活性領域のそれぞれを覆う第2の保護材料を更に含む、請求項1記載の装置。
- 前記カソライト材料が、酸素種を実質的に含まない、請求項1記載の装置。
- 前記カソライトが、ネッキング配置によって相互連結された複数の粒子を含み、粒子直径対ネックの寸法比が、多結晶構造を形成するために1%〜100%超であり、かつ前記正極領域の全体積の30%未満の空隙率を有する、請求項1記載の装置。
- 前記活物質が鉄及びフッ素を含む、請求項1記載の装置。
- 前記活物質が、NCA(ニッケルコバルトアルミニウム酸化物)、LMNO(リチウムマンガンニッケル酸化物)、LCO(リチウムコバルト酸化物、即ち、LiCoO2)、フッ化ニッケル(NiFx、式中xは0〜2.5)、又はフッ化銅(CuFy、式中、yは0〜2.5)から選択される正極材料である、請求項1記載の装置。
- 前記活物質が、CuF2から選択された正極材料である、請求項23記載の装置。
- 前記活物質が、NiF2から選択された正極材料である、請求項23記載の装置。
- 前記カソライトが、LiaSiPbSc又はLiaGePbScのいずれかから選択され;式中、2≦a≦10、0.5≦b≦2.5、4≦c≦12、d<3である、請求項1記載の装置。
- 前記カソライトが、LiaGePbScから選択され;式中、2≦a≦10、0.5≦b≦2.5、4≦c≦12、d<3である、請求項1記載の装置。
- 前記カソライト材料が、Li2S、P2S5、及びGeS2又はSiS2を400〜700℃で約4時間を超えて焼鈍することによって形成される、請求項1記載の装置。
- 前記カソライト材料が、Li2S、P2S5、Ge、及びSを400〜700℃で、約4時間を超えて焼鈍することによって形成される、請求項1記載の装置。
- 前記カソライト材料が、Li2S、P2S5、Si、及びSを400〜700℃で、約4時間を超えて焼鈍することによって形成される、請求項1記載の装置。
- LGPS又はLSPS含有材料内に含められた酸素種を更に含み、該酸素種が、硫黄種に対して1:10以下の比率を有する、請求項1記載の装置。
- 前記活性領域が、前記正極領域の50 vol%を超えている、請求項1記載の装置。
- 前記カソライトが、10-5〜5×10-2 S/cmの室温イオン伝導率、及び10-5 S/cm未満の電気伝導率を有する、請求項1記載の装置。
- 前記室温イオン伝導率が10-4〜1e-2 S/cmであり、かつ前記電気伝導率が10-5 S/cm未満である、請求項33記載の装置。
- 前記カソライトが、LSPSであり、かつ10-5 S/cm〜10-2 S/cmの室温イオン伝導率;
1e-5 S/cm未満の電気伝導率を有し;かつ
Cu Kα放射線を用いたXRD 2θスキャンが、33°±1°、30°±1°、又は43°±1°での主ピークによって特徴付けられる、請求項1記載の装置。 - 前記カソライトが、LSPSであり、かつ10-5 S/cm〜10-2 S/cmの室温イオン伝導率;
1e-5S/cm未満の電気伝導率を有し;かつ
Cu Kα放射線を用いたXRD 2θスキャンが、約41〜45° 2θの第1の主ピーク及び約30〜35° 2θの第2の主ピーク及び51〜54° 2θの第3の主ピークによって特徴付けられる、請求項1記載の装置。 - リチウム元素;
シリコン元素又はゲルマニウム元素;
リン元素;
硫黄元素:
及び酸素元素を含み;
2θ=33°±1°又は2θ=43°±1°でのCu Kα XRD主ピークによって特徴付けられる、固体カソライト材料。 - 式LiaSiPbScOd(式中、2≦a≦8、0.5≦b≦2.5、4≦c≦12、d<3)によって特徴付けられ、全ての不純物が10 at%未満である、請求項37記載の材料。
- レニショーinViaラマンマイクロスコープによって測定すると418±10 cm-1、383±10 cm-1、286±10 cm-1、及び1614±10 cm-1での一次ラマンピークによって特徴付けられる、請求項37記載の材料。
- xのLi2S、yのSiS2、及びzのP2S5(式中、1≦x/y≦50、かつ0.5≦z/y≦3)の反応によって形成される、請求項37記載の材料。
- xのLi2S、yの(Si及びS2)、及びzのP2S5(式中、1≦x/y≦50、かつ0.5≦z/y≦3)の反応によって形成される、請求項37記載の材料。
- 固体カソライト材料を製造する方法であって:
Li2S、P2S5、及びSiS2又は[Si及びS]を混合するステップ;及び該混合物を、400℃を超える温度に3時間を超えて加熱するステップを含む、前記方法。 - 固体カソライト材料を製造する方法であって:
Li2S、P2S5、及びSiS2又は[Ge及びS]を混合するステップ;及び該混合物を、400℃を超える温度に3時間を超えて加熱するステップを含む、前記方法。 - 正極領域を含むエネルギー保存装置であって、該正極領域が:
該正極領域内に空間的に配置された複数の第1の活性領域を含む主活性領域;
該正極領域の空間領域内に空間的に閉じ込められ、かつ該第1の活性領域によって占められていない空間領域内に空間的に配置されたカソライト材料であって、それぞれ多結晶状態又は非晶質状態に構成された、リチウム、ゲルマニウム、リン、及び硫黄(「LGPS」)含有材料、又はリチウム、すず、リン、及び硫黄(「LTPS」)含有材料、又はリチウム、シリコン、リン、及び硫黄(「LSPS」)含有材料を含む、該カソライト材料;
該LGPS、LTPS、又はLSPS含有材料内に含められたドーパント種であって、該LGPS、LTPS、又はLSPS材料のイオン伝導率を第1のイオン伝導率値から第2のイオン伝導率値に上昇させることによって特徴付けられる、該ドーパント種;及び
該LGPS、LTPS、又はLSPS含有材料と正極活物質との間の反応を最小限にするために、該活物質の露出領域を覆うように形成された閉じ込め材料、を含む、前記装置。 - 前記LGPS、LTPS、又はLSPS含有材料内に含められた酸素種を更に含み、該酸素種が、LGPSO、LTPSO、又はLSPSO材料を形成するために硫黄種に対して1:2以下の比率を有し;
該酸素種が、該LGPSO又はLSPSO材料の1%未満〜20%であり;
前記ドーパント種が、すず元素、アルミニウム元素、炭素、チタン、ハフニウム、セリウム、及びジルコニウムから選択される、請求項44記載の装置。 - 前記硫黄含有種が、前記LGPSO又はLSPSO材料の約20〜60%である、請求項44記載の装置。
- 前記主活性領域が、前記正極領域の50 vol%を超えている、請求項44記載の装置。
- 前記カソライト材料が、前記主活性領域を含む前記正極領域を実質的に満たして、該正極領域を画定する実質的に均一な厚さの材料を形成するように構成されている、請求項44記載の装置。
- 前記複数の活性領域がそれぞれ、約20 nm〜約3μmのサイズを有する、請求項44記載の装置。
- 前記カソライト材料が複数のクラスターを含み、該クラスターの大多数が、約10 nm〜約300 nmのメディアン径を有する、請求項44記載の装置。
- 前記カソライト材料が、前記正極活性領域の周りに複数のシェル構造を含む、請求項44記載の装置。
- 前記カソライト材料が複数の粒子として構成され、前記粒子の大多数が、約20 nm〜約1μmのメディアン径を有する、請求項44記載の装置。
- 前記カソライト材料が、酸素種を実質的に含まない、請求項44記載の装置。
- 前記LSPS材料が、LSTPS合金材料を形成するために前記ドーパント種を用いて構成されている、請求項44記載の装置。
- 前記LGPS材料が、LGTPS合金材料を形成するために前記ドーパント種を用いて構成されている、請求項44記載の装置。
- 前記ドーパント種が、第1のドーパント種及び第2のドーパント種を含み;該第1のドーパント種が、該第2のドーパント種とは異なる元素である、請求項44記載の装置。
- リチウム種、シリコン種、リン種、及び硫黄種を含むドープLSPS材料であって、LSTPS合金材料を形成するためにすず種からなる複数のドーパント種を用いて構成され;該リチウム種が30〜50 at%であり;該シリコン種が0〜15 at%であり;該すず種が0〜15 at%であり;該リン種が5〜17 at%であり;該硫黄種が30〜55 at%であり;かつ0〜15 at%の酸素種を更に含む、前記ドープLSPS材料。
- リチウム種、ゲルマニウム種、リン種、及び硫黄種を含むドープLGPS材料であって、LGTPS合金材料を形成するために複数のすず種を用いてドープされ;該リチウム種が30〜50 at%であり;該ゲルマニウム種が0〜15 at%であり;該すず種が0〜15 at%であり;該リン種が5〜17 at%であり;該硫黄種が30〜55 at%であり;かつ0〜15 at%の酸素種を更に含む、前記ドープLGPS材料。
- リチウム種、ゲルマニウム種、リン種、及び硫黄種を含むドープLGPS材料であって、LGSPS合金材料を形成するために複数のドーパント種を用いて形成され;該リチウム種が30〜50 at%であり;該ゲルマニウム種が0〜15 at%であり;シリコン種が0〜15 at%であり;該リン種が5〜17 at%であり;該硫黄種が30〜55 at%であり;かつ0〜15 at%の酸素種を更に含む、前記ドープLGPS材料。
- 18〜21°、26〜28°、28〜31°、40〜42°、及び46〜48°を含む複数の範囲における複数の異なるXRDピークで特徴付けられるドープLiaMPbSc(LMPS)材料であって;MがSi、Ge、Sn、又はこれらの組み合わせから選択される、前記材料。
0.5〜1.5 ppmの少なくとも1つの7LiのNMRピークシフトで特徴付けられるドープLiaMPbSc(LMPS)材料であって;MがSi、Ge、Sn、又はこれらの組み合わせから選択される、前記材料。 - 284 eVでの炭素1sピークに対して校正されたときに58 eV±1 eVでのXPSのリチウムピーク位置によって特徴付けられる、請求項37、55、56、又は57〜58のいずれか一項記載の材料。
- 284 eVでの炭素1sピークに対して校正されたときに104 eV±1 eVでのXPSのリチウムピーク位置によって特徴付けられる、請求項37、55、56、又は57〜58のいずれか一項記載の材料。
- 284 eVでの炭素1sピークに対して校正されたときに134 eV±1 eVでのXPSのリチウムピーク位置によって特徴付けられる、請求項37、55、56、又は57〜58のいずれか一項記載の材料。
- 284 eVでの炭素1sピークに対して校正されたときに164 eV±1 eVでのXPSのリチウムピーク位置によって特徴付けられる、請求項37、55、56、又は57〜58のいずれか一項記載の材料。
- 284 eVでの炭素1sピークに対して校正されたときに533 eV±1 eVでのXPSのリチウムピーク位置によって特徴付けられる、請求項37、55、56、又は57〜58のいずれか一項記載の材料。
- 86〜88 ppm、92〜94 ppm、73〜78 ppm、又は108〜109.5 ppmの少なくとも1つの31PのNMRピークシフトで特徴付けられるドープLiaMPbSc(LMPS)材料であって;MがSi、Ge、Sn、又はこれらの組み合わせから選択される、前記材料。
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KR20220129669A (ko) | 2022-09-23 |
KR102239187B1 (ko) | 2021-04-09 |
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EP2997611A2 (en) | 2016-03-23 |
CN105518906B (zh) | 2019-04-16 |
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US9819024B2 (en) | 2017-11-14 |
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