JP2015176867A - 高い単位面積あたり容量を維持するリチウムイオン電池のためのSi/C複合体アノード - Google Patents
高い単位面積あたり容量を維持するリチウムイオン電池のためのSi/C複合体アノード Download PDFInfo
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 42
- 239000010703 silicon Substances 0.000 title claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 38
- 229910052799 carbon Inorganic materials 0.000 title claims description 21
- 239000002131 composite material Substances 0.000 title claims description 17
- 229910001416 lithium ion Inorganic materials 0.000 title claims description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title description 5
- 230000002459 sustained effect Effects 0.000 title 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000010405 anode material Substances 0.000 claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 18
- 238000000197 pyrolysis Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002153 silicon-carbon composite material Substances 0.000 claims abstract description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 239000002482 conductive additive Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 8
- 229920005596 polymer binder Polymers 0.000 claims abstract description 7
- 239000002491 polymer binding agent Substances 0.000 claims abstract description 7
- 229920002959 polymer blend Polymers 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract 2
- 239000002245 particle Substances 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 18
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 18
- 239000004800 polyvinyl chloride Substances 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 17
- 239000010439 graphite Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 13
- 239000006229 carbon black Substances 0.000 claims description 11
- 229920000620 organic polymer Polymers 0.000 claims description 9
- 239000002174 Styrene-butadiene Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 239000011115 styrene butadiene Substances 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract 2
- 238000003801 milling Methods 0.000 abstract 1
- 239000011149 active material Substances 0.000 description 28
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 13
- 239000000654 additive Substances 0.000 description 11
- 229910052786 argon Inorganic materials 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 239000011856 silicon-based particle Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 229910001413 alkali metal ion Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000005979 thermal decomposition reaction Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- -1 excessive oxygen Chemical compound 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 3
- 239000011246 composite particle Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000006183 anode active material Substances 0.000 description 1
- 150000001485 argon Chemical class 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011263 electroactive material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000006138 lithiation reaction Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012457 nonaqueous media Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
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Abstract
Description
10%径 : ≦1μm
50%径 : ≦5μm
90%径 : ≦15μm
平均直径 : 3〜6μm
より好ましい粒子は、以下の粒径分布を有する粒子である:
10%径 : ≦0.6μm
50%径 : ≦4.0μm
90%径 : ≦11.0μm
平均直径 : 3.5〜5.0μm
最も好ましい粒子は、以下の粒径分布を有する粒子である:
10%径 : 0.45±0.05μm
50%径 : 3.0±0.2μm
90%径 : 10.0±0.5μm
平均直径 : 4.0〜4.5μm
吸収水の除去:約100℃まで加熱し、この温度を約15分保つ。
アニーリング:炭素源が融解するが分解はしない温度、例えばPVCの場合約300℃まで加熱し、この温度を約30分保つ。
熱分解:熱分解が起こる温度、PVCの場合800℃超(例えば830℃)まで加熱し、この温度を約1時間保つ。
加熱速度:4〜7℃/分。
冷却速度:1〜2℃。
A)材料の調製
ケイ素/炭素複合体、活性材料(AM)を2つのステップで調製した。まず、マイクロサイズの商用ケイ素粉末を高分子(炭素源)と共にアニールし、続いて高分子を熱分解して熱分解高分子被覆ケイ素を形成した。次に、ボール粉砕ステップを実施して、所望のサイズ分布を有するケイ素複合体粒子及び炭素質薄片を得た。走査型電子顕微鏡(SEM)によって粉末の形態を検査し、Cilas990レーザ粒径アナライザを用いてサイズ分布を検査した。有機分析はLECO C/H/Nアナライザを用いて実施した。
40〜50%の量のAMと、高分子バインダ(本実施例では3〜25%の量の炭素メチルセルロースバインダ(CMC)及び/又は同様の量のスチレンブタジエン(SBR)バインダ)と、導電性添加剤(本実施例では、好ましくは5〜40%の量のカーボンブラック(Super P(商標) Li Timcal)及び0〜40%の量のグラファイト(SLP50(商標) Timcal))とを用いて電極を調製した。表1は3つの実施例の組成の詳細を示す。AM及び添加剤を水中で均質に混合し、このスラリーを11μmのCu箔上にキャスティングした。更に、電極を真空条件下で90℃において12時間乾燥させた。電極の乾燥後、1.54cm2のコイン状片を打ち抜き、電気化学的試験に用いた。
電極の3つの実施例を調製した。
規格CR2025のコイン型セル技術を用いて、電気化学的試験を実施した。セルを不活性アルゴンで充填したグローブボックス内で組み立て、Li金属箔をステンレス鋼ディスクに押圧したものを対電極として用いて、室温で試験サイクルに供した。商用ポリプロピレンディスク(Celgard 2400)を用いてSi/C電極とLi電極を隔てた。電解質は商用炭酸塩混合溶液(Novolyte SSDE-R-21)であった。セルを、放電レートC/7.5においてLiに対して0.05〜1.5Vの定電流状態において動作させた。結果を図3に示し、熱分解を施していないSi電極の挙動を図7に示す。
同一の活性AMを用いて調製され、AMと添加剤との比が1.2であるケイ素アノードの3つの代表的な実施例から、電極組成は実施例2、実施例3(共にカーボンブラック(Super P)を含有するが、グラファイト(SLP50)を含有しない)に関して同一であったが、実施例1の組成とは、実施例1がカーボンブラック(Super P)及びグラファイト(SLP50)を含有していた点において異なっていた。SLP50の添加により、アノードの機械的安定性に関して妥協することなくAMの積載量を高めることができた。その結果、実施例1の組成では単位面積あたり容量が3.83mAh/cm2となり、これは少なくとも50サイクルにわたって保持された。実施例2のアノードでは単位面積あたり容量は商用グラファイトアノードの範囲内となった。実施例3のアノードは、塗布した厚さの違いにより、その厚さが半分になっているにも関わらず密度は高くなっている点で、同一のスラリーを使用した実施例2のアノードとは異なっていた。
Claims (15)
- 合金化が可能なケイ素炭素複合体電気活性アノード材料(AM)を製造する方法であって:
マイクロサイズのケイ素粉末をマイクロサイズの有機高分子粉末と混合して、ケイ素‐高分子混合物を製造するステップ;
前記ケイ素‐高分子混合物を不活性ガス中で熱分解温度まで加熱し、前記有機高分子が熱分解して熱分解高分子被覆ケイ素を形成するのに十分な長さの時間にわたって、前記熱分解温度の前記不活性ガス中に保つステップ;及び
前記熱分解高分子被覆ケイ素を不活性ガス中で粉砕して、前記ケイ素炭素複合体電気活性アノード材料(AM)を形成するステップ
を含む、方法。 - 前記マイクロサイズのケイ素粉末は、5〜80μm、一般には5〜50μm、好ましくは10〜40μmの粒径を有する、請求項1に記載の方法。
- 前記マイクロサイズの有機高分子粉末は、200μm以下、好ましくは100μm以下の平均粒径を有し、最も好ましくは少なくとも90%の粒子が100μm以下の粒径を有する、請求項1又は2に記載の方法。
- ケイ素と有機高分子との比率は1:2〜3:8、例えば1:2〜1:3、又は約3:7である、請求項1〜3のいずれか1項に記載の方法。
- 前記高分子は、ポリ塩化ビニル、特に平均MWが約43000であり、平均Mnが約22000であるポリ塩化ビニルである、請求項1〜4のいずれか1項に記載の方法。
- 前記熱分解温度は、4〜7℃/分の速度で達成され、及び/又は
前記熱分解温度は、0.5〜2時間保たれる、請求項1〜5のいずれか1項に記載の方法。 - 前記粉砕ステップは、高エネルギボールミル、特に15:1〜30:1、好ましくは20:1のボール/粉末重量比を用いる高エネルギボールミルを用いて、回転速度800〜1200rpmで15分〜4時間、例えば約1000rpmで約20分間、約25℃となるよう温度を制御しながら行われる、請求項1〜6のいずれか1項に記載の方法。
- 炭素質の薄片で覆われた粒子からなるケイ素炭素複合体電気活性アノード材料であって、
前記粒子の10%は≦1μmの直径を有し、前記粒子の50%は≦5μmの直径を有し、前記粒子の90%は≦15μmの直径を有し、前記複合体は3〜6μmの平均直径を有し、
好ましくは、前記粒子の10%は≦0.6μmの粒径を有し、前記粒子の50%は≦4.0μmの粒径を有し、前記粒子の90%は≦11.0μmの粒径を有し、前記複合体は3.5〜5.0μmの平均直径を有し、
より好ましくは、前記粒子の10%は0.45±0.05μmの粒径を有し、前記粒子の50%は3.0±0.2の粒径を有し、前記粒子の90%は10.0±0.5μmの粒径を有し、前記粒子は4.0〜4.5μmの平均直径を有する、ケイ素炭素複合体電気活性アノード材料。 - 請求項1〜7のいずれか1項に記載の方法によって得ることができる、ケイ素炭素複合体電気活性アノード材料。
- 請求項8又は9に記載のケイ素炭素複合体電気活性アノード材料と、高分子バインダ、導電性添加剤、及び好ましくは水である溶媒とを混合してスラリーを形成するステップ、並びに
前記スラリーを集電体に塗布して乾燥させるステップ
を含む、アノードを製造するための方法。 - 前記高分子バインダは、炭素メチルセルロース(CMC)バインダ又はスチレンブタジエン(SBR)バインダ又は好ましくはこれらの混合物からなる群から選択される、請求項10に記載の方法。
- 前記導電性添加剤は、カーボンブラック、グラファイト又はこれらの混合物からなる群から選択され、特にカーボンブラックであり、より好ましくはカーボンブラックとグラファイトの組み合わせである、請求項10又は11に記載の方法。
- 前記高分子バインダは、5〜40%、より好ましくは10〜30%、例えば15〜25%の量で使用され、及び/又は前記導電性添加剤は、合計5〜50%、好ましくは10〜40%、より好ましくは30〜40%の量で使用され、
カーボンブラックとグラファイトとの比は、2:1〜0.5:1、特に約0.9:1〜1.1:1、例えば約1:1である、請求項10〜12のいずれか1項に記載の方法。 - 請求項8又は9に記載のケイ素炭素複合体電気活性アノード材料、高分子バインダ、及び導電性添加剤を含む、電極であって、
特に請求項10〜13のいずれか1項に記載の方法によって得ることができる、電極。 - 請求項14の電極を備える二次電池であって、
特にLiイオン電池である、二次電池。
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