JP7109879B2 - 高容量高分子の陰極および該陰極を含む高エネルギー密度の再充電可能な電池 - Google Patents
高容量高分子の陰極および該陰極を含む高エネルギー密度の再充電可能な電池 Download PDFInfo
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- JP7109879B2 JP7109879B2 JP2016560448A JP2016560448A JP7109879B2 JP 7109879 B2 JP7109879 B2 JP 7109879B2 JP 2016560448 A JP2016560448 A JP 2016560448A JP 2016560448 A JP2016560448 A JP 2016560448A JP 7109879 B2 JP7109879 B2 JP 7109879B2
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- 238000006138 lithiation reaction Methods 0.000 description 1
- 229910001540 lithium hexafluoroarsenate(V) Inorganic materials 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- MCVFFRWZNYZUIJ-UHFFFAOYSA-M lithium;trifluoromethanesulfonate Chemical compound [Li+].[O-]S(=O)(=O)C(F)(F)F MCVFFRWZNYZUIJ-UHFFFAOYSA-M 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910000474 mercury oxide Inorganic materials 0.000 description 1
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000483 nickel oxide hydroxide Inorganic materials 0.000 description 1
- MRHPUNCYMXRSMA-UHFFFAOYSA-N nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Ni++] MRHPUNCYMXRSMA-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000010094 polymer processing Methods 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001472 pulsed field gradient Methods 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 description 1
- RAVDHKVWJUPFPT-UHFFFAOYSA-N silver;oxido(dioxo)vanadium Chemical compound [Ag+].[O-][V](=O)=O RAVDHKVWJUPFPT-UHFFFAOYSA-N 0.000 description 1
- 238000000371 solid-state nuclear magnetic resonance spectroscopy Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- RBYFNZOIUUXJQD-UHFFFAOYSA-J tetralithium oxalate Chemical compound [Li+].[Li+].[Li+].[Li+].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O RBYFNZOIUUXJQD-UHFFFAOYSA-J 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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Description
aterial)の使用(例えば:特許文献1参照)、および2)「硫化」複合陰極物質を生成するために硫黄と反応する伝導性高分子の使用、に焦点を当てた。「硫化高分子」の例は、ポリアクリロニトリル(PAN)と一緒の硫黄の高温暴露からの反応生成物を含む[非特許文献1および2参照]。硫黄陰極に使用される他の伝導性高分子系は、ポリビニルピロリドン(PVP)[非特許文献3参照]およびポリピロール(PPY)[非特許文献4参照]を含む。これらの方法はポリスルフィドのシャトル機序を限定するための様々な程度の成功に遭遇したが、それらはすべて、大規模製造に十分には適さない高価な材料の使用に基づく。
室温および広範な温度範囲の双方において、非常に高いイオン拡散率(diffusivity)および伝導率(conductivity)をもつ固体のイオン伝導性高分子物質が提供される。固体のイオン性高分子物質は、電池の固体電解質として有用であり、更に電池の電極を製造するための構成部品(component)として有用である。その物質は電池の用途に限定はされず、アルカリ燃料電池、スーパーキャパシタ(supercapacitors)、エレクトロクロミック装置(electrochromic
devices)、センサー等のような他の目的のために、より広く適用できる。高分子物質は、他の場合には可燃性である可能性がある用途に対して特に魅力的な、不燃性で、自消性である。更に該物質は機械的に強靭で、それら自体、当該技術分野で知られた大量(high volume)の高分子処理法および装置を使用して製造することができる。
のうちの2成分の混合物を含む、所望のイオン含有化合物に化学的に転化可能なイオンまたは物質を含有する化合物を含む。
して製造される。本明細書で使用される硫黄は、元素の硫黄、高分子の硫黄、黄鉄鉱および、陰極の電気化学反応に対して硫黄を供給するように働くことができる他の物質、のような、電気活性(electroactive)硫黄のあらゆる原料を意味することが意図される。
本出願はそれぞれ、すべての目的のためにその全体が、参照することにより本明細書に組み入れられる、2014年12月3日出願の米国特許出願第14/559,430号明細書および2014年4月1日出願の米国仮出願第61/973,325号明細書に対する優先権を主張する。
一つの態様において、本発明はリチウムイオンを伝導するために電池中に使用される、固体のイオン伝導性高分子物質に関する。
必要としない。
ンレス鋼の電極間に挟まれる。電圧がかけられ、それは酸化方向の安定性に対して高い値(Liに対して4ボルトを超える)まで正の方向に、そして還元方向の安定性に対して、低い値(Liに対して0V以下)に負の方向に移動される(swept)。電極の界面で何か重要な反応が起こるかどうか決定するために電流出力が測定される。高い正の電圧における高い電流出力は、酸化反応が起こっていることを表わすと考えられ、それは、これらの、または、より正の電圧において作動する陰極物質(多数の金属酸化物のような)による不安定を示唆している。低電圧における高い電流出力は、還元反応が起こることを表わし、それはこれらの、またはより負の電圧で作動する陽極(金属Liまたはリチウム化炭素のような)による不安定を示唆すると考えられる。図10は、リチウム金属に対する、本発明に従う固体のイオン伝導性高分子物質を含む固体高分子の電解質に対する、電圧対電流のプロットを示す。その研究は、固体の高分子の電解質が、約4.6ボルトまで安定であることを示す。これらの結果は、固体の高分子の電解質が、非限定的例としてのリン酸鉄および硫黄陰極のような低電圧陰極と一緒に、LCO、LMO、NMCおよび類似の陰極を含む陰極により安定であることができることを示す。
更に、本発明は複合高分子-硫黄の陰極に関する。複合高分子-硫黄の陰極は、硫黄成分並びに、基材高分子、ドーパントおよび、イオン源を含む化合物、を含む固体のイオン伝導性高分子物質を含む。複合高分子-硫黄の陰極は、二次リチウムまたはLiイオン硫黄電池に使用される時に、高い比容量および高い容量保持率をもつことを特徴とする。該複合陰極は200 milliamp-時/gmを超える、そして好適には500 milliamp-時/gmを超える、そしてより好適には750 milliamp-時/
gmを超える、そして最も好適には1000 milliamp-時/gmを超える比容量をもつことを特徴とする。該複合陰極は、500再充電/放電サイクル超に対して、少なくとも50%、そして好適には少なくとも80%の保持率をもつことを特徴とする。本発明の複合高分子-硫黄の陰極は、本複合電極に使用される独特な高分子により可能にされる低コストの、大規模な製造に対する直接の応用をもつ。本発明の複合高分子-硫黄の陰極は、同時に低コストの電池を製造するための条件を満たしながら、高性能(high
performance)を提供することができる。
S8 → Li2S8 → Li2S4 → Li2S2 → Li2S
に示される、系列(sequence)により、連続的に、より低い次元のポリスルフィドを形成する。
うあらゆる他の方法、あるいはプラスチックを加工する(engineering)ための当業者により知られた他の方法、により形成されることができる。
および~2.1Vにおける二つの平坦域(plateaus)を示す。これは、複合高分子-硫黄系が、安定な電気化学的連結と合致する、リチウム/硫黄系に対する期待された電圧曲線を形成しながら、高い容量を可能にすることを示す。
、伝導性フォイル支持体の両面上に、電気活性の固体のイオン伝導性高分子物質-硫黄の混合物で被覆されて、高分子-硫黄の陰極を形成した。これらの陰極は、リチウム金属の陽極(4.9×8.1cm)、ポリプロピレン隔離体および0.5MのLiNO3添加剤を含むDOL/DME電解質中の1MのLiTFSIを使用してパウチ電池(pouch
cell)に組み立てられた。電池は、水および酸素の低い不活性雰囲気のグローブボックスの内部で真空密封された。
高次に織り合わされた(highly ordered interwoven)複合電極の注目すべき例は文献[Ji,X.;Lee,K.T.;Nazar,L.F.Nature Materials 2009,8,500-506]に提示されている。この複合陰極は、155℃の熱処理により孔中に固定された(entrenched)硫黄を伴うCMK-3中間細孔(mesoporous)炭素を使用した。図23は、文献例のLi/硫黄-CMK-3に対する第1の放電を、本発明のLi/複合高分子-硫黄のものと比較している。
リチウム電池の陰極としての硫黄-伝導性高分子複合体の使用が示された。一例において、ポリアクリロニトリル(PAN)を硫化して、伝導性および化学的に活性な陰極物質を形成する。高分子の硫化は、~300℃の、比較的高温で起こる。米国特許出願第2014/0045059号明細書[He,X.-M.,et.al.]に開示された本物質の放電曲線の一例が図24に示される。図24はLi/硫黄-ポリアクリロニトリル(S /PAN)電池に対して認められる、典型的な電圧の特徴(signature)を示す 。これらの電池は2.0V未満の平均電圧により単一の、傾斜する電圧の平坦域を特徴として示す。本発明の電池におけるLi/複合高分子-硫黄の陰極に対して図19に認められた電圧曲線に比較して、S/PAN電池は、放電期間中、有意に、より低い電圧を示し 、それがワット-時に基づく、より低いエネルギー密度をもたらすことが認められる。従 って、本発明の複合高分子-硫黄の陰極により開示される電圧動態は、硫化PAN-基剤 の陰極の動態よりも優れている。
リチウム/硫黄コイン電池のサイクル試験の一例は文献[Urbonaite,S.;
Novak,P.J.Power Sources 2014,249,497-502]に提供されている。その硫黄の陰極は、本発明の陰極に使用された炭素に匹敵する標準の炭素黒物質を使用した。J.Power Sources文献中の電解質、隔離体およびリチウム陽極はすべて、本発明の電池に使用される物質と同一であった。その相異は、J.Power Sources文献中の陰極が、本発明の、固体のイオン伝導性高分子物質を含まなかったことである。従って、本文献の例は、本発明の高分子-電解質を取り入れる陰極を使用する電池に対する良好な対照を提供する。対照のLi/硫黄のコイン電池のサイクル寿命曲線は図25に示される。文献の電池は明白に、1000サイクル超において本発明の電池と同様な容量に対して約500サイクルのみを提供した。従って、本発明の電池は、文献例のサイクル寿命のほぼ2倍を提供した。
Claims (13)
- 硫黄を含む活性物質および固体のイオン伝導性高分子物質を混合したものを含む陰極の電極であって、前記固体のイオン伝導性高分子物質が20℃~26℃の室温で1×10-4S/cmを超えるイオン伝導率を有し、前記固体のイオン伝導性高分子物質が基材高分子と電子受容体とイオン源を含む化合物の反応体生成物から形成されており、ここで、前記基材高分子が共役高分子、ポリフェニレンスルフィド、液晶高分子、ポリエーテルエーテルケトン(PEEK)、30%を超える結晶化度を持つ半晶質高分子および前記の少なくとも2種の組み合わせ物よりなる群から選択され、前記電子受容体がジクロロジシアノキノン(C8Cl2N2O2)、テトラシアノエチレン(TCNE(C6N4))、三酸化硫黄(SO3)、クロラニルおよび前記の少なくとも2種の組み合わせ物よりなる群から選択され、かつ、前記イオン源を含む化合物がLiOH、Li2Oおよび前記の混合物よりなる群から選択される、ことを特徴とする陰極の電極。
- 請求項1に記載の陰極の電極であって、前記基材高分子がポリフェニレンスルフィド、液晶高分子、ポリエーテルエーテルケトン(PEEK)、30%を超える結晶化度を持つ半晶質高分子および前記の少なくとも2種の組み合わせ物よりなる群から選択される、ことを特徴とする陰極の電極。
- 請求項1又は2に記載の陰極の電極であって、前記固体のイオン伝導性高分子物質が室温で1秒当り1×10-11平方メートルを超えるリチウムカチオン拡散率を有する、ことを特徴とする陰極の電極。
- 請求項1又は2に記載の陰極の電極であって、導電率を付加するための導電性充填剤をさらに含む、ことを特徴とする陰極の電極。
- 請求項1又は2に記載の陰極の電極であって、前記固体のイオン伝導性高分子物質が、前記活性物質の少なくとも1粒子をカプセル封入する、ことを特徴とする陰極の電極。
- 請求項1又は2に記載の陰極の電極であって、前記固体のイオン伝導性高分子物質が、電気絶縁性であることを特徴とする陰極の電極。
- 請求項1に記載の陰極の電極であって、前記基材高分子が、Li + 群の存在下で酸化的にドーピングされている、ことを特徴とする陰極の電極。
- 請求項7に記載の陰極の電極であって、前記基材高分子が共役高分子である、
ことを特徴とする陰極の電極。 - 陽極および請求項1又は2に記載の陰極の電極を含む、電気化学的電池。
- 請求項9に記載の電気化学電池であって、前記電気化学電池の電圧が1.0ボルトを超える、ことを特徴とする電気化学電池。
- 請求項9に記載の電気化学電池であって、前記陽極がリチウム、錫、ケイ素、
黒鉛、および前記の少なくとも2種の合金もしくは混合物よりなる群から選択される、ことを特徴とする電気化学電池。 - 請求項9に記載の電気化学電池であって、前記電気化学電池が二次電池である、ことを特徴とする電気化学電池。
- 請求項1又は2に記載の陰極の電極であって、前記基材高分子がポリフェニレンスルフィドであり、前記電子受容体がジクロロジシアノキノン(C8Cl2N2O2)であり、かつ、前記イオン源を含む化合物がLiOHである、ことを特徴とする陰極の電極。
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KR20160143711A (ko) | 2016-12-14 |
CN106489217B (zh) | 2021-07-30 |
EP3127177A4 (en) | 2017-12-27 |
SG11201608197RA (en) | 2016-10-28 |
JP2017517835A (ja) | 2017-06-29 |
EP3127177B1 (en) | 2021-01-06 |
EP3127177A1 (en) | 2017-02-08 |
CN113659140A (zh) | 2021-11-16 |
US20150280218A1 (en) | 2015-10-01 |
JP2023123622A (ja) | 2023-09-05 |
EP3896771A1 (en) | 2021-10-20 |
WO2015153729A1 (en) | 2015-10-08 |
HUE053572T2 (hu) | 2021-07-28 |
CN106489217A (zh) | 2017-03-08 |
JP2020184545A (ja) | 2020-11-12 |
US20210288313A1 (en) | 2021-09-16 |
KR102385977B1 (ko) | 2022-04-13 |
PL3127177T3 (pl) | 2021-06-14 |
WO2015153729A8 (en) | 2016-11-10 |
US20210257609A9 (en) | 2021-08-19 |
US11145857B2 (en) | 2021-10-12 |
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