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すなわち本発明は、以下の発明を提供するものである。
（１）リチウムイオンを吸蔵および放出可能な正極と、リチウムイオンを吸蔵および放出可能な負極と、前記正極と前記負極との間に配置されたセパレータとを有し、リチウムイオン伝導性を有する非水電解液中に、前記正極と前記負極と前記セパレータとを設けた非水電解質二次電池であって、前記負極の負極活物質は、元素Ｘを含む第１の粒子と、元素Ｍを含む第２の粒子とを含み、前記元素Ｘは、Ｓｉ、Ｓｎ、Ａｌ、Ｐｂ、Ｓｂ、Ｂｉ、Ｇｅ、Ｉｎ、Ｚｎからなる群より選ばれた１種の元素であって、前記元素Ｍが、第４〜１１族の遷移金属元素からなる群より選ばれた少なくとも１種の元素であって、前記第１の粒子は、前記元素Ｘの単体または元素Ｘを主成分とする固溶体からなり、前記第２の粒子は、前記元素Ｍの単体または化合物からなり、前記電解液は、分子内に不飽和結合を有し還元重合が可能な有機物を０．１重量％〜１０重量％含有していることを特徴とする非水電解質二次電池。
（２）前記第１の粒子の平均粒径が２ｎｍ〜５００ｎｍであり、前記第２の粒子の平均粒径が２ｎｍ〜１０μｍであることを特徴とする（１）に記載の非水電解質二次電池。
（３）前記負極において、前記第１の粒子の表面と、前記第２の粒子の表面とは１μｍ以内にあることを特徴とする（１）または（２）に記載の非水電解質二次電池。
（４）リチウムイオンを吸蔵および放出可能な正極と、リチウムイオンを吸蔵および放出可能な負極と、前記正極と前記負極との間に配置されたセパレータとを有し、リチウムイオン伝導性を有する非水電解液中に、前記正極と前記負極と前記セパレータとを設けた非水電解質二次電池であって、前記負極の負極活物質は、元素Ｘと元素Ｍとを含むナノサイズ粒子からなり、前記元素Ｘは、Ｓｉ、Ｓｎ、Ａｌ、Ｐｂ、Ｓｂ、Ｂｉ、Ｇｅ、Ｉｎ、Ｚｎからなる群より選ばれた１種の元素であって、前記元素Ｍが、第４〜１１族の遷移金属元素からなる群より選ばれた少なくとも１種の元素であって、前記ナノサイズ粒子は、前記元素Ｘの単体または元素Ｘを主成分とする固溶体である第１の相と、前記元素Ｍの単体、元素Ｍを主成分とする固溶体または元素Ｍの化合物である第２の相と、を少なくとも有し、前記ナノサイズ粒子は、前記第１の相と前記第２の相との両方が外表面に露出するととともに、界面を介して接合しており、前記第１の相は、外表面が略球面状であり、前記ナノサイズ粒子は、平均粒径が２ｎｍ〜５００ｎｍであり、前記電解液は、分子内に不飽和結合を有し還元重合が可能な有機物を０．１重量％〜１０重量％含有することを特徴とする非水電解質二次電池。
（５）前記ナノサイズ粒子は、Ｃｕ、Ｆｅ、Ｃｏ、Ｎｉ、Ｃａ、Ｓｃ、Ｔｉ、Ｖ、Ｃｒ、Ｍｎ、Ｓｒ、Ｙ、Ｚｒ、Ｎｂ、Ｍｏ、Ｔｃ、Ｒｕ、Ｒｈ、Ｂａ、ランタノイド元素（ＣｅおよびＰｍを除く）、Ｈｆ、Ｔａ、Ｗ、Ｒｅ、Ｏｓ、Ｉｒからなる群より選ばれた少なくとも１種の元素である元素Ｍ’をさらに含み、前記元素Ｍ’が、前記第２の相を構成する前記元素Ｍとは種類の異なる元素であり、前記元素Ｍ’の単体または化合物である他の第２の相をさらに有していることを特徴とする（４）に記載の非水電解質二次電池。
（６）前記ナノサイズ粒子は、Ｓｉ、Ｓｎ、Ａｌ、Ｐｂ、Ｓｂ、Ｂｉ、Ｇｅ、Ｉｎ、Ｚｎからなる群より選ばれた少なくとも１種の元素である元素Ｘ’をさらに含み、前記元素Ｘ’の単体または固溶体である第３の相をさらに有していることを特徴とする（４）または（５）に記載の非水電解質二次電池。
（７）前記第３の相が、前記第１の相と前記第２の相の少なくとも一方と、界面を介して接合していることを特徴とする（６）記載の非水電解質二次電池。
（８）前記第１の粒子が、（４）〜（７）のいずれかに記載のナノサイズ粒子であることを特徴とする（１）〜（３）のいずれかに記載の非水電解質二次電池。
（９）前記分子内に不飽和結合を有し還元重合が可能な有機物が、フルオロエチレンカーボネート、ビニレンカーボネート及びその誘導体、ビニルエチレンカーボネートからなる群より選ばれた少なくとも１種であることを特徴とする（１）〜（８）のいずれかに記載の非水電解質二次電池。
（１０）前記負極は、少なくとも、負極活物質、導電材および結着材を含む塗布液が、集電体に塗布され、乾燥されて形成されることを特徴とする（１）〜（９）のいずれかに記載の非水電解質二次電池。
That is, the present invention provides the following inventions.
(1) a positive electrode capable of inserting and extracting lithium ions, a negative electrode capable of inserting and extracting lithium ions, and a separator disposed between the positive electrode and the negative electrode, and having lithium ion conductivity A non-aqueous electrolyte secondary battery in which the positive electrode, the negative electrode, and the separator are provided in an aqueous electrolyte, wherein the negative electrode active material of the negative electrode includes first particles containing an element X and an element M And the element X is one element selected from the group consisting of Si, Sn, Al, Pb, Sb, Bi, Ge, In, and Zn, and the element M is: At least one element selected from the group consisting of transition metal elements of Groups 4 to 11, wherein the first particles are composed of the element X alone or a solid solution containing the element X as a main component , The second particle is the element M or a single element. Made from the object, the electrolyte is a nonaqueous electrolyte secondary battery, characterized by reducing polymerizing an unsaturated bond in the molecule contains organics 0.1% to 10% by weight possible.
(2) The nonaqueous electrolyte secondary according to (1), wherein the average particle diameter of the first particles is 2 nm to 500 nm, and the average particle diameter of the second particles is 2 nm to 10 μm. battery.
(3) The nonaqueous electrolyte secondary battery according to (1) or (2), wherein the surface of the first particle and the surface of the second particle are within 1 μm in the negative electrode. .
(4) having a positive electrode capable of inserting and extracting lithium ions, a negative electrode capable of inserting and extracting lithium ions, and a separator disposed between the positive electrode and the negative electrode, and having a lithium ion conductivity In the nonaqueous electrolyte secondary battery in which the positive electrode, the negative electrode, and the separator are provided in a water electrolyte, the negative electrode active material of the negative electrode is composed of nano-sized particles containing the element X and the element M, The element X is one element selected from the group consisting of Si, Sn, Al, Pb, Sb, Bi, Ge, In, and Zn, and the element M is a transition metal of group 4 to 11 At least one element selected from the group consisting of elements, wherein the nano-sized particles are a single phase of the element X or a solid solution containing the element X as a main component; and a simple element of the element M , Solid solution mainly composed of element M Or has a second phase which is a compound of the element M, at least, the nano-sized particles, with the both the first phase and the second phase is exposed on the outer surface, through the interface The first phase has a substantially spherical outer surface, the nano-sized particles have an average particle diameter of 2 nm to 500 nm, and the electrolyte has an unsaturated bond in the molecule. A non-aqueous electrolyte secondary battery comprising 0.1% by weight to 10% by weight of an organic substance capable of reduction polymerization.
(5) The nano-sized particles include Cu, Fe, Co, Ni, Ca, Sc, Ti, V, Cr, Mn, Sr, Y, Zr, Nb, Mo, Tc, Ru, Rh, Ba, and a lanthanoid element ( Further including an element M ′, which is at least one element selected from the group consisting of Hf, Ta, W, Re, Os, and Ir, and the element M ′ includes the second phase. The non-water according to ( 4), wherein the element M constituting the element is a different type of element and further has another second phase that is a simple substance or a compound of the element M ′. Electrolyte secondary battery.
(6) The nano-sized particles further include an element X ′ that is at least one element selected from the group consisting of Si, Sn, Al, Pb, Sb, Bi, Ge, In, and Zn. The nonaqueous electrolyte secondary battery according to (4) or (5) , further comprising a third phase which is a simple substance or a solid solution.
(7) The nonaqueous electrolyte secondary battery according to ( 6 ), wherein the third phase is bonded to at least one of the first phase and the second phase via an interface. .
(8) The non-aqueous electrolyte 2 according to any one of (1) to (3), wherein the first particles are nano-sized particles according to any one of (4) to ( 7 ). Next battery.
(9) The organic substance having an unsaturated bond in the molecule and capable of reductive polymerization is at least one selected from the group consisting of fluoroethylene carbonate, vinylene carbonate and derivatives thereof, and vinyl ethylene carbonate. The nonaqueous electrolyte secondary battery according to any one of (1) to ( 8 ).
(10) The negative electrode is formed by applying a coating liquid containing at least a negative electrode active material, a conductive material, and a binder to a current collector, and drying the coating solution (1) to ( 9 ) The nonaqueous electrolyte secondary battery according to any one of the above.
第２の粒子１０は、元素Ｍの単体からなってもよいし、元素Ｍの化合物からなってもよい。ここで、元素Ｍは、周期律表の第４〜１１族の遷移金属元素からなる群より選ばれた少なくとも１種の元素であり、例えば、第４〜１１族の遷移金属元素のうち、安定な元素、具体的には、Ｔｉ、Ｖ、Ｃｒ、Ｍｎ、Ｆｅ、Ｃｏ、Ｎｉ、Ｃｕ、Ｚｒ、Ｎｂ、Ｍｏ、Ｒｕ、Ｒｈ、Ｐｄ、Ａｇ、Ｈｆ、Ｔａ、Ｗ、Ｒｅ、Ｏｓ、Ｉｒ、Ｐｔ、Ａｕ等である。これらの元素Ｍは、リチウムを吸蔵しにくい元素である。元素Ｍと化合物を形成する元素については、特に制限されないが、前記の元素Ｘとすることもできる。第２の粒子１０は、ほとんどリチウム吸蔵特性を示さないが、元素Ｍの割合や、化合物を形成する元素により、リチウム吸蔵特性を調整することもできる。また、化合物とは、各種の合金、金属間化合物、酸化物等を含むことができる。
The second particles 10 may be composed of the element M alone or a compound of the element M. Here, the element M is at least one element selected from the group consisting of group 4 to group 11 transition metal elements of the periodic table. For example, among the group 4 to group 11 transition metal elements, the element M is stable. Elements such as Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Hf, Ta, W, Re, Os, Ir, Pt, Au, etc. These elements M are elements that do not easily store lithium. The element that forms a compound with the element M is not particularly limited, but may be the element X described above. The second particles 10 hardly exhibit lithium storage characteristics, but the lithium storage characteristics can be adjusted by the ratio of the element M and the elements forming the compound. The compound can include various alloys, intermetallic compounds, oxides, and the like.
また、第２の相１５は、元素Ｍの単体であってもよいし、または元素Ｍを主成分とする固溶体であってもよく、元素Ｍの化合物であってもよい。この第２の相１５は、リチウムをほとんど吸蔵しない。また、元素Ｍは、上記のとおり、ｄ電子軌道に２以上の多くの電子が存在していることから、負極５を保護する皮膜の形成を促進して、サイクル特性を向上させることができる。
In addition, the second phase 15 may be a single element M, a solid solution containing the element M as a main component, or a compound of the element M. The second phase 15 hardly absorbs lithium. In addition, since the element M has two or more electrons in the d electron orbit as described above, the formation of a film that protects the negative electrode 5 can be promoted and cycle characteristics can be improved.
（ナノサイズ粒子の評価）
実施例１〜４、比較例１に係るＳｉ系ナノサイズ粒子において、実施例１に示す方法で、６３．７ＭＰａで粉体粒子を圧縮した条件で測定した粉体導電率を、表１に示す。
実施例１〜４は、粉体導電率が４×１０−８［Ｓ／ｃｍ］以上であり、比較例１は粉体導電率が４×１０−８[Ｓ／ｃｍ]未満を示した。なお、比較例１は、測定限界である１×１０−８[Ｓ／ｃｍ]未満であった。粉体導電率が高いと導電助剤の配合を少なくすることができ、電極の単位体積当りの容量を高くすることができるとともに、ハイレート特性で有利となる。
(Evaluation of nano-sized particles)
Table 1 shows the powder conductivity measured for the Si-based nano-sized particles according to Examples 1 to 4 and Comparative Example 1 under the condition that the powder particles were compressed at 63.7 MPa by the method shown in Example 1. .
In Examples 1 to 4, the powder conductivity was 4 × 10 −8 [S / cm] or more, and in Comparative Example 1, the powder conductivity was less than 4 × 10 −8 [S / cm]. In Comparative Example 1, the measurement limit was less than 1 × 10 −8 [S / cm]. When the powder conductivity is high, the blending of the conductive auxiliary agent can be reduced, the capacity per unit volume of the electrode can be increased, and it is advantageous in high rate characteristics.
Claims (10)
前記負極の負極活物質は、元素Ｘを含む第１の粒子と、元素Ｍを含む第２の粒子とを含み、
前記元素Ｘは、Ｓｉ、Ｓｎ、Ａｌ、Ｐｂ、Ｓｂ、Ｂｉ、Ｇｅ、Ｉｎ、Ｚｎからなる群より選ばれた１種の元素であって、
前記元素Ｍが、第４〜１１族の遷移金属元素からなる群より選ばれた少なくとも１種の元素であって、
前記第１の粒子は、前記元素Ｘの単体または元素Ｘを主成分とする固溶体からなり、
前記第２の粒子は、前記元素Ｍの単体または化合物からなり、
前記電解液は、分子内に不飽和結合を有し還元重合が可能な有機物を０．１重量％〜１０重量％含有している
ことを特徴とする非水電解質二次電池。 A non-aqueous electrolyte having a lithium ion conductivity, having a positive electrode capable of inserting and extracting lithium ions, a negative electrode capable of inserting and extracting lithium ions, and a separator disposed between the positive electrode and the negative electrode A non-aqueous electrolyte secondary battery in which the positive electrode, the negative electrode, and the separator are provided,
The negative electrode active material of the negative electrode includes first particles containing the element X and second particles containing the element M,
The element X is one element selected from the group consisting of Si, Sn, Al, Pb, Sb, Bi, Ge, In, and Zn,
The element M is at least one element selected from the group consisting of Group 4 to 11 transition metal elements,
The first particle is composed of the element X alone or a solid solution containing the element X as a main component ,
The second particles are composed of a single element or a compound of the element M,
The non-aqueous electrolyte secondary battery, wherein the electrolytic solution contains 0.1 wt% to 10 wt% of an organic substance having an unsaturated bond in a molecule and capable of reduction polymerization.
前記負極の負極活物質は、元素Ｘと元素Ｍとを含むナノサイズ粒子からなり、
前記元素Ｘは、Ｓｉ、Ｓｎ、Ａｌ、Ｐｂ、Ｓｂ、Ｂｉ、Ｇｅ、Ｉｎ、Ｚｎからなる群より選ばれた１種の元素であって、
前記元素Ｍが、第４〜１１族の遷移金属元素からなる群より選ばれた少なくとも１種の元素であって、
前記ナノサイズ粒子は、前記元素Ｘの単体または元素Ｘを主成分とする固溶体である第１の相と、前記元素Ｍの単体、元素Ｍを主成分とする固溶体または元素Ｍの化合物である第２の相と、を少なくとも有し、
前記ナノサイズ粒子は、前記第１の相と前記第２の相との両方が外表面に露出するととともに、界面を介して接合しており、前記第１の相は、外表面が略球面状であり、
前記ナノサイズ粒子は、平均粒径が２ｎｍ〜５００ｎｍであり、
前記電解液は、分子内に不飽和結合を有し還元重合が可能な有機物を０．１重量％〜１０重量％含有する
ことを特徴とする非水電解質二次電池。 A non-aqueous electrolyte having a lithium ion conductivity, having a positive electrode capable of inserting and extracting lithium ions, a negative electrode capable of inserting and extracting lithium ions, and a separator disposed between the positive electrode and the negative electrode A non-aqueous electrolyte secondary battery in which the positive electrode, the negative electrode, and the separator are provided,
The negative electrode active material of the negative electrode is composed of nano-sized particles containing the element X and the element M,
The element X is one element selected from the group consisting of Si, Sn, Al, Pb, Sb, Bi, Ge, In, and Zn,
The element M is at least one element selected from the group consisting of Group 4 to 11 transition metal elements,
The nano-sized particles are a first phase that is a single element of the element X or a solid solution that contains the element X as a main component, and a single solution of the element M, a solid solution that contains the element M as a main component, or a compound of the element M. Two phases, and
The nano-sized particles have both the first phase and the second phase exposed to the outer surface and bonded via an interface, and the outer surface of the first phase is substantially spherical. And
The nano-sized particles have an average particle diameter of 2 nm to 500 nm,
The electrolyte solution contains 0.1 wt% to 10 wt% of an organic substance having an unsaturated bond in the molecule and capable of reductive polymerization.
前記元素Ｍ’が、前記第２の相を構成する前記元素Ｍとは種類の異なる元素であり、
前記元素Ｍ’の単体または化合物である他の第２の相をさらに有している
ことを特徴とする請求項４に記載の非水電解質二次電池。 The nano-sized particles are Cu, Fe, Co, Ni, Ca, Sc, Ti, V, Cr, Mn, Sr, Y, Zr, Nb, Mo, Tc, Ru, Rh, Ba, lanthanoid elements (Ce and Pm). And an element M ′ that is at least one element selected from the group consisting of Hf, Ta, W, Re, Os, and Ir,
The element M ′ is an element different in kind from the element M constituting the second phase,
The nonaqueous electrolyte secondary battery according to claim 4, further comprising another second phase that is a single element or a compound of the element M ′.
前記元素Ｘ’の単体または固溶体である第３の相をさらに有している
ことを特徴とする請求項４または請求項５に記載の非水電解質二次電池。 The nano-sized particles further include an element X ′ that is at least one element selected from the group consisting of Si, Sn, Al, Pb, Sb, Bi, Ge, In, and Zn,
The non-aqueous electrolyte secondary battery according to claim 4 or claim 5, characterized in that it further includes a single or third phase is a solid solution of the element X '.
The negative electrode, at least, the negative electrode active material, a coating solution containing a conductive material and a binder material, is applied to the current collector, any one of claims 1 to 9, characterized in that it is formed by dry The non-aqueous electrolyte secondary battery described in 1.
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| JP2010250223A JP5520782B2 (en) | 2010-11-08 | 2010-11-08 | Nonaqueous electrolyte secondary battery |
| PCT/JP2011/075564 WO2012063765A1 (en) | 2010-11-08 | 2011-11-07 | Non-aqueous electrolyte secondary battery |
| KR1020137012990A KR101520557B1 (en) | 2010-11-08 | 2011-11-07 | Non-aqueous electrolyte secondary battery |
| CN201180053949.2A CN103222092B (en) | 2010-11-08 | 2011-11-07 | Rechargeable nonaqueous electrolytic battery |
| TW100140677A TWI437746B (en) | 2010-11-08 | 2011-11-08 | Non-aqueous electrolyte secondary battery |
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| JP6629402B2 (en) * | 2013-09-18 | 2020-01-15 | 株式会社東芝 | Positive electrode |
| JP6400391B2 (en) * | 2013-09-18 | 2018-10-03 | 株式会社東芝 | Non-aqueous electrolyte battery |
| JP6427878B2 (en) * | 2014-01-14 | 2018-11-28 | 東ソー株式会社 | Si-based negative electrode material and method for producing the same |
| CN105489840B (en) * | 2016-01-13 | 2018-06-19 | 哈尔滨工业大学深圳研究生院 | A kind of Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method thereof |
| JP6659504B2 (en) * | 2016-09-20 | 2020-03-04 | 株式会社東芝 | Solid electrolyte, lithium battery, battery pack, and vehicle |
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| KR20060010727A (en) * | 2003-05-22 | 2006-02-02 | 마쯔시다덴기산교 가부시키가이샤 | Nonaqueous electrolyte secondary battery and method for producing same |
| JP2005197080A (en) * | 2004-01-07 | 2005-07-21 | Nec Corp | Anode for secondary battery and secondary battery using it |
| JP4078338B2 (en) * | 2004-04-20 | 2008-04-23 | 三洋電機株式会社 | Electrode for lithium secondary battery and lithium secondary battery |
| CN100367545C (en) * | 2004-04-20 | 2008-02-06 | 三洋电机株式会社 | Electrode for lithium secondary cell and lithium secondary cell thereof |
| JP4051686B2 (en) * | 2004-09-30 | 2008-02-27 | ソニー株式会社 | Negative electrode active material and battery using the same |
| JP5560736B2 (en) * | 2009-01-30 | 2014-07-30 | 株式会社エクォス・リサーチ | Fuel cell |
| JP5484816B2 (en) * | 2009-08-03 | 2014-05-07 | 古河電気工業株式会社 | Negative electrode material for lithium ion secondary battery containing nano-sized particles, negative electrode for lithium ion secondary battery, lithium ion secondary battery |
| JP5520538B2 (en) * | 2009-08-03 | 2014-06-11 | 古河電気工業株式会社 | Negative electrode material for lithium ion secondary battery containing nano-sized particles, negative electrode for lithium ion secondary battery, lithium ion secondary battery |
| JP5598836B2 (en) * | 2009-08-03 | 2014-10-01 | 古河電気工業株式会社 | Negative electrode material for lithium ion secondary battery containing nano-sized particles, negative electrode for lithium ion secondary battery, lithium ion secondary battery |
-
2010
- 2010-11-08 JP JP2010250223A patent/JP5520782B2/en active Active
-
2011
- 2011-11-07 CN CN201180053949.2A patent/CN103222092B/en not_active Expired - Fee Related
- 2011-11-07 WO PCT/JP2011/075564 patent/WO2012063765A1/en active Application Filing
- 2011-11-07 KR KR1020137012990A patent/KR101520557B1/en not_active IP Right Cessation
- 2011-11-08 TW TW100140677A patent/TWI437746B/en not_active IP Right Cessation
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