JP7505783B2 - ケイ素-炭素複合アノード材料 - Google Patents
ケイ素-炭素複合アノード材料 Download PDFInfo
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- JP7505783B2 JP7505783B2 JP2021526291A JP2021526291A JP7505783B2 JP 7505783 B2 JP7505783 B2 JP 7505783B2 JP 2021526291 A JP2021526291 A JP 2021526291A JP 2021526291 A JP2021526291 A JP 2021526291A JP 7505783 B2 JP7505783 B2 JP 7505783B2
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Images
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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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Description
実施例1a:太陽電池からのSiの回収
この調製において使用されるケイ素は、第1世代太陽光(PV)パネル(すなわち、単結晶または多結晶ケイ素を含む)の使用されなくなった太陽電池を回収することで得たが、Siが他の供給源からも同様に得られ得ることは明らかであろう。
Si粉末(125μm未満)を、1.5mmのジルコニアビーズを使用して遊星ボールミル粉砕機内で1時間にわたってボールミル粉砕した。無水イソプロパノールを溶媒として添加して、プロセスにおいてSiの最小限の酸化を確実にした。得られた懸濁液におけるSiの濃度は、40重量%であった。その後、今回は0.5mmのジルコニアビーズを使用して、懸濁液を3時間にわたってさらにボールミル粉砕した。
Si/C複合粒子(すなわち、二次粒子)を、導電性炭素としてのカーボンブラック(CB)(Alfa Aesar、カーボンブラック、アセチレン、100%圧縮、99.9+%)およびバインダーとしてのカルボキシメチルセルロース(CMC)(Sigma Aldrich)と、pH3のKOHおよびクエン酸の水性緩衝液中でさらに混合して、スラリーを得た。Si/C:CB:CMCの重量比は、1:1:1であった。
Si/C複合材料層を完全に乾燥させたら、水(0.4重量%)中に入った酸化グラフェン(GO)懸濁液(Graphenea、スペイン)をフィルムの上部にキャスティングし、続いて、室温で一晩かけて乾燥させた。乾燥した懸濁液によって、1μmまでの厚さを有するGO層のスタックを形成することができた。それによって、目的の複合アノード材料を得た。
次いで、乾燥した複合アノード材料を15mmのディスクに切断し、アルゴンを充填したグローブボックス内にてコイン電池内で組み立てた。ここでは、複合アノード材料電極によって1つの半電池を形成し、金属リチウムを対極および参照電極として使用し、電解質は、固形物(すなわち、電極)/電解質中間相(SEI)を安定化させるための添加剤としての10重量%のフルオロエチレンカーボネート(FEC)および2重量%のビニレンカーボネート(VC)と一緒にエチレンカーボネート(EC)およびジメチルカーボネート(DMC)中に入ったLiPF6であった。
実施例2a:全容量での実施例1の複合アノード材料の電気化学的性能
複合アノード材料の電気化学的性能を、実施例1eによるコイン電池の0.01~1Vの電圧範囲内で、定電流サイクルによって調べた。ここでは、印加した電流密度(Cレート)を、変換反応に関与する3個のLiの理論容量(すなわち、3600mAh/g)に基づいて計算した。電池をC/20の低電流で定電流充放電によってまず速度論的に安定化させた。
得られた容量および保持値をWO2016/106487のものと比較すると、WO2016/106487のバッテリに印加された電流密度(0.3A/g=C/12)が本実施例より低くても、報告された可逆容量(110サイクル後に約1800mAh/g)および容量保持率(110サイクル後に78.3%)が劣っていることが分かる。この点において、通常、電流密度が低いほど、電気化学反応がより低い速度で起こることが可能になり、したがって、(例えば、反応が速度論的に何らかの制限を受けている場合に)バッテリの初期容量に達する機会がより多くなることに言及する価値がある。
実用的なリチウムイオンバッテリにおけるSiの使用に関する重要な態様の1つは、Siがアノードの役割を果たしていることである。したがって、全電池の容量は、カソード材料(すなわち、リチウム供給源)の容量にも依存する。結果的に、ここでのカソード材料の制限に基づいて、Siの理論容量に達する必要はない。したがって、サイクル中にSiと反応するLi+の数を制限して、バッテリにおけるSiの高い容量を維持しながら、形成される合金における体積膨張を減らした。反応するリチウムの数を1個に制限することによって、1200mAh/gのSiの理論容量を得る。この制限は、バッテリの充放電に費やされる電流密度および全時間に適用された。
ここで、図9および図10を参照する。2つのサンプルのうちの1つについてはGO層のキャスティングを省略したことを除いて、2つのサンプルを実施例1で説明したように調製した。GO層を有しないサンプルの形態は、図9に示されており、GO層を有するサンプルは、図10に示されている。
ここで、図12を参照する。比較のために、サンプルを、実施例1で説明したように、ただし噴霧乾燥の代わりに回転蒸発を使用して調製し、その電気化学的性能を図12に示す。C/5での350サイクルにわたる初期容量および容量保持率は、噴霧乾燥によって調製された均質に混合されたSi/C複合粒子に基づくものよりも明らかに良好ではなかった。したがって、一般に、噴霧乾燥法が好ましい。回転蒸発器内で調製された粒子は凝集体を形成する傾向があり、それによって、Li拡散が制限され得ることが観察された。
実施例3a
実施例1を繰り返したが、太陽電池ではなく、ドープされていないSiウェハ断片をSi供給源として使用した。この場合、一般に、最初に断片から金属を浸出させる必要はなかった。したがって、125μm未満の粒径を有するSi粉末を得るために、予備破砕のみを実施する必要があった。
実施例1を繰り返したが、市販のSiナノ粉末をSi供給源として使用した。この場合、一般に、浸出ステップまたは予備破砕ステップは必要ではなかった。さらに、ボールミル粉砕ステップは、PVPとCNT添加剤とを混合するためにのみ使用され、それによって、噴霧乾燥のための懸濁液が得られた。
実施例1を繰り返したが、噴霧乾燥のための懸濁液を形成するために、CNT(すなわち、導電性炭素)懸濁液のみをSi一次粒子に添加した。
実施例1を繰り返したが、噴霧乾燥のための懸濁液を形成するために、PVP(すなわち、有機化合物)溶液のみをSi一次粒子に添加した。
実施例1および3a~dで使用される異なる成分、ならびにこれらの複合アノード材料について得られた電気化学的結果を、以下の表に要約する。
本発明による複合アノード材料をKイオンバッテリ内の負極材料として調べた。ケイ素は、1個のカリウムとだけ反応して、K/K+に対して平均電圧0.15Vで954mAh/gの理論容量をもたらすことができるが、我々の知る限りでは、そのような値は、まだ実験的には得られていない。むしろ、ほとんどの研究では、200mAh/g未満の容量が得られ、これらの容量を数サイクルしか維持することができない。
実施例4を繰り返すが、金属ナトリウム(Na)を対極および参照電極として使用し、好適なNa系電解質を使用する。同等の結果が得られる。
Claims (15)
- i.ケイ素-炭素複合粒子を含むケイ素-炭素複合材料層と、
ii.前記ケイ素-炭素複合材料層を覆う酸化グラフェン層と、
を含み、前記ケイ素-炭素複合粒子がそれぞれ、炭素系材料と混合された複数のケイ素粒子を含む、複合アノード材料において、
前記ケイ素-炭素複合粒子が、中空部を取り囲む多孔質シェルを含み、前記多孔質シェルが、前記炭素系材料と混合された前記複数のケイ素粒子を含むことを特徴とする、複合アノード材料。 - 前記ケイ素-炭素複合材料層が、
ia.以下のものからのマトリックスと:
-導電性炭素材料、および
-バインダー
ib.前記マトリックス中に分散したケイ素-炭素複合粒子と、を含む、請求項1に記載の複合アノード材料。 - 前記炭素系材料が導電性炭素材料である、請求項1または2に記載の複合アノード材料。
- 前記ケイ素-炭素複合粒子が、少なくとも80重量%のSi含有量を有する、請求項1~3のいずれか1項に記載の複合アノード材料。
- 前記ケイ素-炭素複合材料が前記酸化グラフェン層の上方に存在しないことを条件とする、請求項1~4のいずれか1項に記載の複合アノード材料。
- 請求項1~5のいずれか1項に記載の複合アノード材料を形成する方法であって、
a.ケイ素-炭素複合粒子を含むケイ素-炭素複合材料層を提供することと、
b.前記ケイ素-炭素複合材料層の上方に酸化グラフェン層を提供することと、
を含み、ステップaの前に、
a’1.200nm以下の平均サイズを有するケイ素粒子の懸濁液を提供することと、
a’2.炭素系材料をケイ素粒子の前記懸濁液に混合することと、
a’3.ケイ素粒子と炭素系材料との前記懸濁液を噴霧乾燥させてケイ素-炭素複合粒子を形成することと、
a’4.還元雰囲気で前記ケイ素-炭素複合粒子を焼成することと、を含む前記ケイ素-炭素複合粒子を形成するステップa’を含む、方法。 - ステップaで前記ケイ素-炭素複合材料層を提供することが、
a1.導電性基板上に前記ケイ素-炭素複合材料のスラリーを提供することと、
a2.前記スラリーを乾燥させて前記ケイ素-炭素複合材料層を形成することと、を含む、請求項6に記載の方法。 - ステップa1で前記導電性基板上にケイ素-炭素複合材料の前記スラリーを提供することが、
-前記ケイ素-炭素複合粒子を導電性炭素材料およびバインダーと混合して前記スラリーを形成することと、
-ウェットコーティング技術を使用して前記導電性基板上に前記スラリーをコーティングすることと、を含む、請求項7に記載の方法。 - ステップbで前記酸化グラフェン層を提供することが、
b1.前記ケイ素-炭素複合材料層上に酸化グラフェンの水性懸濁液を提供することと、
b2.前記水性懸濁液を乾燥させて前記酸化グラフェン層を形成することと、を含む、請求項6~8のいずれか1項に記載の方法。 - ステップa2および/またはb2(存在する場合)が、150℃以下の温度で実施される、請求項9に記載の方法。
- ステップa’1および/またはステップa’2がボールミル粉砕を含む、請求項6~10のいずれか1項に記載の方法。
- 前記ケイ素粒子が、太陽電池および/またはウェハ断片から得られる、請求項6~11のいずれか1項に記載の方法。
- ステップaが、ステップbの開始前に完了される、請求項6~12のいずれか1項に記載の方法。
- 請求項1~5のいずれか1項に記載の複合アノード材料を含む、バッテリ。
- リチウムイオンバッテリ、カリウムイオンバッテリ、またはナトリウムイオンバッテリである、請求項14に記載のバッテリ。
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CA3117764A1 (en) | 2020-05-22 |
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EP3654413A1 (en) | 2020-05-20 |
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