JPWO2019198351A1 - 非水電解質二次電池 - Google Patents
非水電解質二次電池 Download PDFInfo
- Publication number
- JPWO2019198351A1 JPWO2019198351A1 JP2020513102A JP2020513102A JPWO2019198351A1 JP WO2019198351 A1 JPWO2019198351 A1 JP WO2019198351A1 JP 2020513102 A JP2020513102 A JP 2020513102A JP 2020513102 A JP2020513102 A JP 2020513102A JP WO2019198351 A1 JPWO2019198351 A1 JP WO2019198351A1
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- JP
- Japan
- Prior art keywords
- positive electrode
- lithium
- active material
- electrode active
- aqueous electrolyte
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011255 nonaqueous electrolyte Substances 0.000 title claims abstract description 55
- 239000007774 positive electrode material Substances 0.000 claims abstract description 96
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 54
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000002131 composite material Substances 0.000 claims abstract description 39
- 239000000654 additive Substances 0.000 claims abstract description 36
- 230000000996 additive effect Effects 0.000 claims abstract description 36
- 229910052751 metal Inorganic materials 0.000 claims abstract description 36
- 239000002184 metal Substances 0.000 claims abstract description 33
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 22
- 150000002739 metals Chemical class 0.000 claims abstract description 14
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 9
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 9
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 claims abstract description 5
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000010703 silicon Substances 0.000 claims description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 9
- CASZBAVUIZZLOB-UHFFFAOYSA-N lithium iron(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Li+] CASZBAVUIZZLOB-UHFFFAOYSA-N 0.000 claims description 5
- 229910002102 lithium manganese oxide Inorganic materials 0.000 claims description 4
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 claims description 4
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- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 150000003983 crown ethers Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
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- 230000001419 dependent effect Effects 0.000 description 1
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- SXWUDUINABFBMK-UHFFFAOYSA-L dilithium;fluoro-dioxido-oxo-$l^{5}-phosphane Chemical compound [Li+].[Li+].[O-]P([O-])(F)=O SXWUDUINABFBMK-UHFFFAOYSA-L 0.000 description 1
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
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- QKBJDEGZZJWPJA-UHFFFAOYSA-N ethyl propyl carbonate Chemical compound [CH2]COC(=O)OCCC QKBJDEGZZJWPJA-UHFFFAOYSA-N 0.000 description 1
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- SDAXRHHPNYTELL-UHFFFAOYSA-N heptanenitrile Chemical compound CCCCCCC#N SDAXRHHPNYTELL-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
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- 229940006487 lithium cation Drugs 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- IGILRSKEFZLPKG-UHFFFAOYSA-M lithium;difluorophosphinate Chemical compound [Li+].[O-]P(F)(F)=O IGILRSKEFZLPKG-UHFFFAOYSA-M 0.000 description 1
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- RCIJMMSZBQEWKW-UHFFFAOYSA-N methyl propan-2-yl carbonate Chemical compound COC(=O)OC(C)C RCIJMMSZBQEWKW-UHFFFAOYSA-N 0.000 description 1
- KKQAVHGECIBFRQ-UHFFFAOYSA-N methyl propyl carbonate Chemical compound CCCOC(=O)OC KKQAVHGECIBFRQ-UHFFFAOYSA-N 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
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- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
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- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- 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
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- 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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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
Description
実施形態の一例である非水電解質二次電池は、正極と、負極と、非水電解質と、セパレータと、電池ケースとを備える。具体的には、正極及び負極がセパレータを介して巻回されてなる巻回型の電極体と、非水電解質とが電池ケースに収容された構造を有する。電極体は、巻回型の電極体に限定されず、正極及び負極がセパレータを介して積層されてなる積層型の電極体など、他の形態の電極体が適用されてもよい。
正極は、例えば金属箔等の正極集電体と、正極集電体上に設けられ、正極活物質及び正極添加剤を含む正極活物質層とで構成される。正極集電体には、アルミニウムなどの正極の電位範囲で安定な金属の箔、当該金属を表層に配置したフィルム等を用いることができる。
本実施形態に係る非水電解質二次電池に用いられる正極活物質は、リチウムと、リチウム以外の金属の総量に対して50モル%以上のニッケルとを含むLiNi複合酸化物を主成分として含む。ここで「主成分として含む」とは、正極活物質の総量に対する第1複合酸化物の含有量が、例えば90質量%以上、好ましくは99質量%以上であることである。
本実施形態に係る非水電解質二次電池では、正極活物質とともに逆蛍石型構造を有するLi含有酸化物で構成される正極添加剤を正極に使用する。これにより、放電末期における負極電位の上昇を抑え、負極の耐久性を向上させることができる。逆蛍石型結晶構造とは、負電荷を有するアニオンによって構成される面心立方格子の四面体サイトに正電荷を有するカチオンが入る結晶構造である。すなわち、単位格子あたり4個のアニオンで構成されており、かつ最大で8個のカチオンの原子が入り得る。逆蛍石型構造としては、例えば、空間群Fm3mに属する結晶構造が挙げられる。
正極活物質層に含まれる導電材の例としては、カーボンブラック、アセチレンブラック、ケッチェンブラック及び黒鉛等の炭素材料等が挙げられる。これらは、単独で用いてもよく、2種類以上を組み合わせて用いてもよい。導電材の含有量は、正極活物質層(正極活物質、正極添加剤、導電材及び結着材)の総量に対して、例えば0.1質量%以上20質量%以下であればよく、0.1質量%以上10質量%以下が好ましい。
正極活物質層に含まれる結着材の例としては、ポリテトラフルオロエチレン(PTFE)及びポリフッ化ビニリデン(PVdF)等のフッ素系樹脂、ポリアクリロニトリル(PAN)、ポリイミド系樹脂、アクリル系樹脂、並びに、ポリオレフィン系樹脂等が挙げられる。結着材は、単独で用いてもよく、2種類以上を組み合わせて用いてもよい。また、これらの結着材に、カルボキシメチルセルロース(CMC)又はその塩(CMC−Na、CMC−K、CMC−NH4等、また部分中和型の塩であってもよい)、ポリエチレンオキシド(PEO)等を併用してもよい。結着剤の含有量は、正極活物質層(正極活物質、正極添加剤、導電材及び結着材)の総量に対して、例えば0.1質量%以上20質量%以下であればよく、0.1質量%以上10質量%以下が好ましい。
負極は、例えば金属箔等の負極集電体と、負極集電体の表面に形成された負極活物質層とを備える。負極集電体には、銅などの負極の電位範囲で安定な金属の箔、銅などの負極の電位範囲で安定な金属を表層に配置したフィルム等を用いることができる。負極活物質層は、リチウムイオンを吸蔵・脱離可能な負極活物質の他に、結着材を含むことが好適である。結着材は増粘剤と併用されてもよい。
非水電解質は、非水溶媒と、非水溶媒に溶解した電解質塩とを含む。
セパレータには、例えば、イオン透過性及び絶縁性を有する多孔性シート等が用いられる。多孔性シートの具体例としては、微多孔薄膜、織布、不織布等が挙げられる。セパレータの材質としては、ポリエチレン、ポリプロピレン等のオレフィン系樹脂、セルロース等が好適である。セパレータは、セルロース繊維層及びオレフィン系樹脂等の熱可塑性樹脂繊維層を有する積層体であってもよい。また、ポリエチレン層及びポリプロピレン層を含む多層セパレータであってもよく、セパレータの表面にアラミド系樹脂等の樹脂が塗布されたものを用いてもよい。
[正極活物質の作製]
NiSO4、CoSO4及びAl2(SO4)3を水溶液中で混合して共沈させることにより、Ni0.88Co0.09Al0.03(OH)2の組成式で表されるニッケルコバルトアルミニウム複合水酸化物を得た。それを焼成して、ニッケルコバルトアルミニウム複合酸化物を作製した。次に、当該複合酸化物と、炭酸リチウムとをらいかい乳鉢を用いて混合した。この混合物における、リチウムと、リチウム以外の金属(Ni、Co、Al)との混合比(モル比)は1.03:1.0であった。更に、リチウム以外の金属(Ni、Co、Al)に対してSiが1モル%となる量のSiOを、当該混合物に加えた。この混合物を空気中において900℃で10時間焼成した後、粉砕することにより、Siを含有するLiNi複合酸化物からなる正極活物質a1を作製した。
<測定条件>
試験温度:常温(25℃)
試験装置:微小圧縮試験機、株式会社島津製作所製、形式名「MCT−W201」
上部加圧圧子:直径50μmの平面
測定モード:圧縮試験
試験荷重:90mN
負荷速度:2.6478mN/秒
炭酸リチウムと、Fe2O3で表される酸化物とを、LiとLi以外の金属元素(Fe)のモル比が5:1になるようにらいかい乳鉢にて混合した。当該混合物を窒素雰囲気中にて600℃で12時間熱処理した後、粉砕することにより、Li含有酸化物からなる正極添加剤b1を作製した。
正極活物質a1と、正極添加剤b1を100:1.5の質量比で混合した後、この正極活物質混合体と、カーボンブラックと、ポリフッ化ビニリデン(PVDF)とを、100:1:1の質量比で混合した。当該混合物に分散媒としてN−メチル−2−ピロリドン(NMP)を添加して混練し、正極合材スラリーを調製した。次に、正極集電体であるアルミニウム箔の表面に正極合材スラリーを塗布し、塗膜を乾燥させた後、圧延ローラにより圧延した。このようにして、アルミニウム箔の両面に正極活物質層が形成された正極を作製した。
黒鉛と、カルボキシメチルセルロース(CMC)と、スチレン−ブタジエンゴム(SBR)とを、100:1:1の質量比で混合し、水を添加した。これを混合機(プライミクス製、T.K.ハイビスミックス)を用いて攪拌し、負極合材スラリーを調製した。次に、負極集電体である銅箔の表面に負極合材スラリーを塗布し、塗膜を乾燥させた後、圧延ローラにより圧延した。このようにして、銅箔の両面に負極活物質層が形成された負極を作製した。
エチレンカーボネート(EC)と、メチルエチルカーボネート(MEC)と、ジメチルカーボネート(DMC)を、30:30:40の体積比(室温)で混合した。当該混合溶媒に、調製後の非水電解質における濃度が1.3モル/Lとなる量のLiPF6を溶解させ、さらに、調製後の非水電解質における濃度が0.3質量%となる量のビニレンカーボネートを溶解させて、非水電解質を調製した。
上記の正極及び負極をそれぞれ所定の寸法にカットした後、上記正極にアルミニウムリードを、上記負極にニッケルリードをそれぞれ取り付けた。ポリエチレン製の微多孔膜をセパレータとして用い、セパレータを介して正極及び負極を渦巻き状に巻回することにより巻回型の電極体を作製した。この電極体を、外径18mm、高さ65mmの有底円筒形状の電池ケース本体に収容し、上記非水電解質を注入した後、ガスケット及び封口体により電池ケース本体の開口部を封口して、18650型の円筒形非水電解質二次電池を作製した。これを実施例1の電池A1と称する。
ニッケルコバルトアルミニウム複合酸化物と炭酸リチウムとの混合物にSiOを添加しなかったこと以外は、実施例1の正極活物質a1の作製方法と同様にして、Siを含有しないNi−Co−Al系の第1複合酸化物a2(正極活物質)を作製した。ICP発光分析法による元素分析の結果、正極活物質a2は組成式Li1.1Ni0.88Co0.09Al0.03O2で表されるLiNi複合酸化物で構成されていた。レーザ回折散乱式粒度分布測定装置(株式会社堀場製作所製)を用いて測定した結果、正極活物質a2の体積平均粒径は11μmであった。また、正極活物質a2の圧縮破壊強度(St)は110MPaであった。
正極の作製において、正極活物質a1に換えて正極活物質a2を使用したこと以外は実施例1と同様にして、円筒形非水電解質二次電池(電池B2)を作製した。
正極の作製において、正極活物質a1と、カーボンブラックと、ポリフッ化ビニリデン(PVDF)とを、100:1:1の質量比で混合して得られる混合物を使用し、正極添加剤b1を使用しなかったこと以外は実施例1と同様にして、円筒形非水電解質二次電池(電池B3)を作製した。
上記で作製した実施例1の電池A1、比較例1〜3の電池B1〜B3を用いて、25℃の温度条件下、充放電電流1It(1Itは電池容量を1時間で放電する電流値であり、ここでは1Itを3000mAとする)、充電終止電圧4.1V、放電終止電圧3Vで充放電を1回行った。この1サイクル目の放電時の放電容量を測定した。次いで、25℃の温度条件下、充放電電流1It、充電終止電圧4.1V、放電終止電圧3Vでの充放電サイクル試験を50回行い、50サイクル目の放電時の放電容量を測定した。
Claims (6)
- 正極と、負極と、非水電解質とを備える非水電解質二次電池であって、
前記正極は、正極集電体と、前記正極集電体の表面に設けられ、正極活物質及び正極添加剤を含む正極活物質層とを有し、
前記正極活物質は、リチウム以外の金属の総量に対して50モル%以上のニッケルを含み、かつ、圧縮破壊強度が130MPa以上であるリチウムニッケル複合酸化物を含有し、
前記正極添加剤は、逆蛍石型構造を有するリチウム含有金属酸化物を含有する、非水電解質二次電池。 - 前記正極添加剤の前記正極活物質層に対する含有量が0.5質量%以上5質量%以下である、請求項1に記載の非水電解質二次電池。
- 前記リチウム含有金属酸化物が、リチウム鉄酸化物、リチウム銅酸化物及びリチウムマンガン酸化物からなる群より選択される少なくとも1つを含む、請求項1又は2に記載の非水電解質二次電池。
- 前記リチウム含有金属酸化物がLi5FeO4である、請求項3に記載の非水電解質二次電池。
- 前記正極活物質がケイ素を更に含有する、請求項1〜4のいずれか一項に記載の非水電解質二次電池。
- 前記ケイ素の含有量が、前記リチウムニッケル複合酸化物に含まれるリチウム以外の金属の総量に対して0.1モル%以上5モル%以下である、請求項5に記載の非水電解質二次電池。
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