JP2019517729A - 金属硫化物ナノ粒子を含むリチウム−硫黄電池用正極活物質及びこの製造方法 - Google Patents
金属硫化物ナノ粒子を含むリチウム−硫黄電池用正極活物質及びこの製造方法 Download PDFInfo
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- JP2019517729A JP2019517729A JP2018563903A JP2018563903A JP2019517729A JP 2019517729 A JP2019517729 A JP 2019517729A JP 2018563903 A JP2018563903 A JP 2018563903A JP 2018563903 A JP2018563903 A JP 2018563903A JP 2019517729 A JP2019517729 A JP 2019517729A
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- Prior art keywords
- lithium
- positive electrode
- sulfur
- active material
- electrode active
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 34
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- 239000011593 sulfur Substances 0.000 claims description 63
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- ZHGDJTMNXSOQDT-UHFFFAOYSA-N NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O Chemical compound NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O ZHGDJTMNXSOQDT-UHFFFAOYSA-N 0.000 description 1
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- 239000002174 Styrene-butadiene Substances 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- BEKPOUATRPPTLV-UHFFFAOYSA-N [Li].BCl Chemical compound [Li].BCl BEKPOUATRPPTLV-UHFFFAOYSA-N 0.000 description 1
- XAQHXGSHRMHVMU-UHFFFAOYSA-N [S].[S] Chemical compound [S].[S] XAQHXGSHRMHVMU-UHFFFAOYSA-N 0.000 description 1
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
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- 229910021525 ceramic electrolyte Inorganic materials 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910052730 francium Inorganic materials 0.000 description 1
- BLBBMBKUUHYSMI-UHFFFAOYSA-N furan-2,3,4,5-tetrol Chemical compound OC=1OC(O)=C(O)C=1O BLBBMBKUUHYSMI-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 229920003049 isoprene rubber Polymers 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- ACFSQHQYDZIPRL-UHFFFAOYSA-N lithium;bis(1,1,2,2,2-pentafluoroethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)C(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)C(F)(F)F ACFSQHQYDZIPRL-UHFFFAOYSA-N 0.000 description 1
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 239000012811 non-conductive material Substances 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000005373 porous glass Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- BUVBYQUZAIPDHT-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S.NC(N)=S BUVBYQUZAIPDHT-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- MDCWDBMBZLORER-UHFFFAOYSA-N triphenyl borate Chemical compound C=1C=CC=CC=1OB(OC=1C=CC=CC=1)OC1=CC=CC=C1 MDCWDBMBZLORER-UHFFFAOYSA-N 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/42—Sulfides or polysulfides of magnesium, calcium, strontium, or barium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/70—Compounds containing carbon and sulfur, e.g. thiophosgene
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H—ELECTRICITY
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
Description
本発明による金属硫化物ナノ粒子は酸化還元の媒介体(Redox mediator)であって、一種の触媒として作用する。本発明による金属硫化物ナノ粒子は、その粒子のサイズによって水分散が可能である。酸化還元の媒介体(Redox mediator)として金属硫化物ナノ粒子を適用すると、ポリスルフィドが炭素表面で電解液または負極の方へ拡散されずに吸着される。この時、触媒作用によって電子伝達が容易となって、固体上の湧出されないLi2S2またはLi2Sに還元される反応が促進され、全体的な硫黄の放電反応(還元反応)の反応速度(Kinetics)が速くなって、湧出されるポリスルフィドの量が減少する。
本発明の炭素−硫黄複合体は、非伝導性の硫黄物質に導電性を与えるためのもので、炭素(C)系物質と硫黄(S)粒子の結合体であり、多孔性の炭素系物質に硫黄粒子が担持された形状であることが好ましい。
上記硫黄/炭素複合体と上記金属硫化物ナノ粒子は、混合されて正極活物質として製造可能である。
図1は、本発明のリチウム−硫黄電池の概略的な断面図である。本発明の一実施例として、リチウム−硫黄電池は上述した正極組成物を含むリチウム−硫黄電池用正極;負極活物質としてリチウム金属またはリチウム合金を含む負極;上記正極と負極の間に介在される分離膜;及び上記負極、正極及び分離膜に含浸されていて、リチウム塩と有機溶媒を含む電解質を含んでもよい。
反応物としてC2H5NS(Thioacetamide:TAA)20mmolとSDS0.4mmolを100mlエタノールに溶かした後、ヒドラジン(Hydrazine)0.2gを添加した。Co(NO3)2・6H2O 10mmolをエタノール120mlに溶かした溶液をTAA混合溶液にゆっくり添加した後、78℃で15時間反応させた。合成された粒子を水とエタノールで3回洗浄した後、遠心分離して70℃で4時間乾燥し、約50nmの粉末粒子を収得した。
上記製造例1のエタノールの代わりにDI−waterを使用して製造例1と同様の方法で約50nmの粉末粒子を収得した。
反応物としてNa2S・9H2O 15mmolをDI−water 75mlに溶かした溶液にCo(NO3)2・6H2O 5mmolをDI−water 75mlに溶かした溶液をゆっくり添加した後、常温で15時間反応させた。以後、製造例1と同様の方法で約50nmの粉末粒子を収得した。
CoCl2・6H2O 2.83gとNa2S2O3 3.16gを蒸溜水50mLに溶解させた後、耐圧容器に入れて140℃で12時間反応させる。以後、溶液を収去してvacuum filtration及びウォッシングした後、60℃で乾燥して約1〜2μmの粉末を得た。上記得られたCoS2マイクロ粒子のSEMイメージを図5に図示す。
改質された炭素粉末(CNT)と硫黄(Sulfur)粉末をボール−ミーリング(Ball−milling)して粉砕した後、155℃のオーブンで30分間置いて、硫黄/炭素複合体を製造した。デンカブラック(Denka black)0.2gとカルボキシメチルセルロース(CMC)分散液5gを入れ、上記製造例1で製造されたCoS2ナノ粒子を10wt%添加してジルコニアボール(Ball)と一緒に混合する。以後、上記製造された硫黄/炭素複合体3.6gと水を一定量入れて再度混合する。最後に、SBRを0.35g入れて再び混合してスラリーを製造した。
上記製造例2で製造されたCoS2ナノ粒子を使用して、上記実施例1と同様の方法でスラリーを製造した。
上記製造例3で製造されたCoS2ナノ粒子を使用して、上記実施例1と同様の方法でスラリーを製造した。
上記CoS2ナノ粒子を添加しないことを除いて、上記実施例1と同様の方法でスラリーを製造した。
上記比較製造例1で製造されたCoS2マイクロ粒子を使用して、上記実施例1と同様の方法でスラリーを製造した。
アルミニウムホイルの上に上記実施例1ないし3、比較例1及び2で製造されたスラリーを注いで、ブレードコーターで一定厚さでコーティングした後、50℃のオーブンで乾燥し、リチウム−硫黄電池用正極を製作した。上記正極をコインセルの大きさに合わせて打ち抜き、アルゴン雰囲気のグローブボックスで組立てる。ステンレススチールの下板に正極、分離膜(Polyethylene)、リチウム負極、ガスケット、ステンレススチールコイン、スプリング、ステンレススチール上板を順に載せ、圧力をかけてコインセルを組立てた。電解液は、1MのLiFSIと1wt%のLiNO3が溶解された1,3−ジオキソラン(1,3−dioxolane:DOL)、ジエチレングリコールジメチルエーテル(Diethylene glycol dimethyl ether:DEGDME)混合液を打ち抜かれた正極の上に注液して使用した。
Claims (10)
- 硫黄/炭素複合体;及び
金属硫化物ナノ粒子を含むリチウム−硫黄電池用正極活物質。 - 前記金属硫化物ナノ粒子は、MxSy(ただし、0<x≦5であり、0<y≦5の整数)で表される化合物であり、Mは、コバルト(Co)、モリブデン(Mo)、チタン(Ti)、ニッケル(Ni)、銅(Cu)、鉄(Fe)、カドミウム(Cd)、鉛(Pb)、マンガン(Mn)、アンチモン(Sb)、ヒ素(As)、銀(Ag)及び水銀(Hg)からなる群から選択された1種以上の金属であることを特徴とする請求項1に記載のリチウム−硫黄電池用正極活物質。
- 前記金属硫化物ナノ粒子の平均粒径は、0.1ないし200nmであることを特徴とする請求項1に記載のリチウム−硫黄電池用正極活物質。
- 前記金属硫化物ナノ粒子は、正極活物質総重量を基準として1ないし20重量%で含まれることを特徴とする請求項1に記載のリチウム−硫黄電池用正極活物質。
- 硫黄/炭素複合体に金属硫化物ナノ粒子を混合して製造する請求項1に記載のリチウム−硫黄電池用正極活物質の製造方法であって、
前記金属硫化物ナノ粒子の製造方法は、
i)硫黄前駆体溶液及び金属前駆体溶液を準備する段階;
ii)前記硫黄前駆体溶液及び金属前駆体溶液を混合する段階;
iii)前記混合溶液を50ないし100℃で5ないし24時間反応させる段階;
iv)前記溶液を洗浄及び精製する段階;及び
v)乾燥する段階;を含むことを特徴とするリチウム−硫黄電池用正極活物質の製造方法。 - 前記硫黄前駆体溶液は、チオアセトアミド(Thioacetamide:TAA)、チオウレア(Thiourea)、硫化ナトリウム(Sodium sulfide、Na2S)からなる群から選択された1種以上の化合物が溶媒に溶解されたことを特徴とする請求項5に記載のリチウム−硫黄電池用正極活物質の製造方法。
- 前記硫黄前駆体溶液は、界面活性剤を含むことを特徴とする請求項5に記載のリチウム−硫黄電池用正極活物質の製造方法。
- 前記金属前駆体溶液は、コバルト(Co)、モリブデン(Mo)、チタン(Ti)、ニッケル(Ni)、銅(Cu)、鉄(Fe)、カドミウム(Cd)、鉛(Pb)、マンガン(Mn)、アンチモン(Sb)、ヒ素(As)、銀(Ag)及び水銀(Hg)からなる群から選択される金属を1種以上含む、アセテート、ヒドロキシド、ナイトレート、ナイトライド、サルフェート、スルフィド、アルコキシド及びハロゲン化物からなる群から選択された1種以上の化合物を含む溶液であることを特徴とする請求項5に記載のリチウム−硫黄電池用正極活物質の製造方法。
- 請求項1ないし4のいずれか一項に記載の正極活物質を含むリチウム−硫黄電池用正極。
- 正極;負極;及び電解質;を含むリチウム−硫黄電池において、
前記正極は、請求項9に記載の正極であることを特徴とするリチウム−硫黄電池。
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