JP5749339B2 - リチウムイオン二次電池 - Google Patents
リチウムイオン二次電池 Download PDFInfo
- Publication number
- JP5749339B2 JP5749339B2 JP2013517836A JP2013517836A JP5749339B2 JP 5749339 B2 JP5749339 B2 JP 5749339B2 JP 2013517836 A JP2013517836 A JP 2013517836A JP 2013517836 A JP2013517836 A JP 2013517836A JP 5749339 B2 JP5749339 B2 JP 5749339B2
- Authority
- JP
- Japan
- Prior art keywords
- secondary battery
- lithium ion
- ion secondary
- oxide particles
- iron oxide
- 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.)
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims description 72
- 229910001416 lithium ion Inorganic materials 0.000 title claims description 72
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 167
- 239000002245 particle Substances 0.000 claims description 109
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 61
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 61
- 239000007773 negative electrode material Substances 0.000 claims description 57
- 239000011148 porous material Substances 0.000 claims description 33
- 229910000859 α-Fe Inorganic materials 0.000 claims description 25
- 239000010410 layer Substances 0.000 claims description 21
- 239000011230 binding agent Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 13
- 239000008151 electrolyte solution Substances 0.000 claims description 10
- 239000003575 carbonaceous material Substances 0.000 claims description 9
- 229910002588 FeOOH Inorganic materials 0.000 claims description 8
- 239000011247 coating layer Substances 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 2
- 229910014630 LixSiyOz Inorganic materials 0.000 claims 1
- 239000000843 powder Substances 0.000 description 90
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 46
- 239000012071 phase Substances 0.000 description 29
- 238000010438 heat treatment Methods 0.000 description 26
- 238000006243 chemical reaction Methods 0.000 description 22
- 229910052744 lithium Inorganic materials 0.000 description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
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- 239000002243 precursor Substances 0.000 description 7
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 239000007864 aqueous solution Substances 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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- 229910015015 LiAsF 6 Inorganic materials 0.000 description 1
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- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910001228 Li[Ni1/3Co1/3Mn1/3]O2 (NCM 111) Inorganic materials 0.000 description 1
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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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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- 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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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Description
リチウムイオン二次電池に用いられる負極活物質は、主として、珪素酸化物からなる珪素酸化物粒子と鉄酸化物からなる鉄酸化物粒子との混合物を含む。以下に、珪素酸化物粒子および鉄酸化物粒子について説明する。なお、本明細書では、珪素酸化物粉末および鉄酸化物粉末と記載することもあるが、いずれも、粒子の集合体としての呼称である。
非結晶性のSiO粉末を含む酸化珪素粉末をミリングすることでも、SiOが不均化して二相に分離する。ミリングの機械的エネルギーの一部が、粒子の固相界面における化学的な原子拡散に寄与し、SiO2相とSi相などを生成すると考えられる。酸化珪素粉末を、真空中、アルゴンガス中などの不活性ガス雰囲気下で、V型混合機、ボールミル、アトライタ、ジェットミル、振動ミル、高エネルギーボールミル等を使用してミリングするとよい。ミリング後にさらに熱処理を施すことで、珪素酸化物の不均化をさらに促進させてもよい。
本発明のリチウムイオン二次電池の負極は、上記の珪素酸化物粒子および鉄酸化物粒子の混合物を負極活物質として含み、集電体と、集電体上に結着された活物質層と、を有する。活物質層は、負極活物質と、導電助剤と、バインダー樹脂と、必要に応じ適量の有機溶剤を加えて混合しスラリーにしたものを、ロールコート法、ディップコート法、ドクターブレード法、スプレーコート法、カーテンコート法などの方法で集電体上に塗布し、バインダー樹脂を硬化させることによって作製することができる。
2SiO+8.6Li++8.6e−→1.5Li4.4Si+1/2Li4SiO4
2SiO+7.35Li++7.35e−→1.42Li4Si+1/3Li2SiO3+1/4Li4SiO4
上記した負極を用いる本発明のリチウムイオン二次電池は、特に限定されない公知の正極、電解質、セパレータを用いることができる。正極は、リチウムイオン二次電池で使用可能なものであればよい。正極は、集電体と、集電体上に結着された正極活物質層とを有する。正極活物質層は、正極活物質と、バインダーとを含み、さらには導電助剤を含んでもよい。正極活物質、導電助材およびバインダーは、特に限定はなく、リチウムイオン二次電池で使用可能なものであればよい。
集電体は、アルミニウム、ニッケル、ステンレス鋼など、リチウムイオン二次電池の正極に一般的に使用されるものであればよい。導電助剤は上記の負極で記載したものと同様のものが使用できる。
平均長さが0.65μm、平均径が0.15μmの棒状粒子からなるα−FeOOH粉末を前駆体として用い、α−Fe2O3を製造した。熱処理は、所定の温度で大気中10時間行った。熱処理温度は、270℃、360℃、500℃または750℃とした。
なお、平均長さおよび平均径は、SEM像より複数の棒状粒子の長さおよび径を実測し、平均した値とした。
低温低湿物理吸着によるBET法(吸着質:窒素)を用い、α−FeOOH粉末および種々の温度で熱処理して得られたα−Fe2O3粉末の比表面積および細孔容積を測定した。結果を図3に示した。図3において、●で示す値は比表面積、□で示す値は細孔容積である。なお、図3において熱処理温度が「0℃」の位置には、未処理のα−FeOOH粉末の測定結果を参考として示した。
鉄酸化物粉末としてα−FeOOH粉末を360℃で熱処理して得たα−Fe2O3粉末を用いて、負極を作製した。
上記の手順で作製した9種類の電極を評価極として用い、9種類のリチウムイオン二次電池(ハーフセル)を作製した。対極は、金属リチウム箔(厚さ500μm)とした。
作製したそれぞれのリチウムイオン二次電池に対し、室温下で充放電試験を行った。
棒状の鉄酸化物粉末または球状の鉄酸化物粉末を用いて、2種類の負極を作製した。棒状の鉄酸化物粉末には、上記のα−FeOOH粉末を360℃で熱処理して得たα−Fe2O3粉末(平均長さ:0.65μm、平均径:0.15μm(アスペクト比:4.3))を用いた。球状の鉄酸化物粉末には、市販のα−Fe2O3粉末(平均粒径:0.7μm(アスペクト比は略1))を用いた。
Claims (11)
- 負極と正極と電解液とを有するリチウムイオン二次電池であって、
前記負極は、負極活物質と結着剤とを有する負極活物質層を有し、
前記負極活物質は、珪素酸化物からなる球状の珪素酸化物粒子と、鉄酸化物からなる棒状の鉄酸化物粒子と、の混合物を含み、
前記混合物全体を100質量%としたとき、前記珪素酸化物粒子を85質量%以上90質量%以下含むことを特徴とするリチウムイオン二次電池。 - 前記鉄酸化物粒子は、表面に複数の細孔を備える請求項1に記載のリチウムイオン二次電池。
- 前記鉄酸化物粒子は、アスペクト比が2以上10以下である請求項1または2に記載のリチウムイオン二次電池。
- 前記鉄酸化物粒子は、平均長さが0.4〜0.7μm、平均径が0.085〜0.17μmである請求項1〜3のいずれかに記載のリチウムイオン二次電池。
- 前記鉄酸化物粒子は、α−Fe2O3を含む請求項1〜4のいずれかに記載のリチウムイオン二次電池。
- 前記鉄酸化物粒子の前記細孔は、FeOOHの熱分解による脱水反応により形成される請求項2に記載のリチウムイオン二次電池。
- 前記珪素酸化物粒子は、SiO2相とSi相とを含み、該SiO2相にはLixSiyOz(0≦x≦4、0.3≦y≦1.6、2≦z≦4)で表される酸化物系化合物が含まれている請求項1〜6のいずれかに記載のリチウムイオン二次電池。
- 前記珪素酸化物粒子は、表面に炭素材料からなる被覆層を備える請求項1〜7のいずれかに記載のリチウムイオン二次電池。
- 前記混合物全体を100質量%としたとき、前記鉄酸化物粒子を5〜15質量%含む請求項1〜8のいずれかに記載のリチウムイオン二次電池。
- 前記鉄酸化物粒子の比表面積は、30m2/g以上1000m2/g以下である請求項1〜9のいずれかに記載のリチウムイオン二次電池。
- 前記鉄酸化物粒子の細孔容積は、0.08cm3/g以上1.0cm3/g以下である請求項2に記載のリチウムイオン二次電池。
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