JP2014139915A - リチウム二次電池 - Google Patents
リチウム二次電池 Download PDFInfo
- Publication number
- JP2014139915A JP2014139915A JP2013130666A JP2013130666A JP2014139915A JP 2014139915 A JP2014139915 A JP 2014139915A JP 2013130666 A JP2013130666 A JP 2013130666A JP 2013130666 A JP2013130666 A JP 2013130666A JP 2014139915 A JP2014139915 A JP 2014139915A
- Authority
- JP
- Japan
- Prior art keywords
- lithium secondary
- secondary battery
- negative electrode
- battery
- sio
- 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
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 114
- 239000011255 nonaqueous electrolyte Substances 0.000 claims abstract description 63
- -1 phosphono acetate chemical compound Chemical class 0.000 claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- VDFVNEFVBPFDSB-UHFFFAOYSA-N 1,3-dioxane Chemical compound C1COCOC1 VDFVNEFVBPFDSB-UHFFFAOYSA-N 0.000 claims abstract description 28
- 125000005843 halogen group Chemical group 0.000 claims abstract description 4
- 125000001183 hydrocarbyl group Chemical group 0.000 claims abstract 2
- 239000003575 carbonaceous material Substances 0.000 claims description 64
- 239000000203 mixture Substances 0.000 claims description 46
- 239000002131 composite material Substances 0.000 claims description 23
- 239000007773 negative electrode material Substances 0.000 claims description 22
- 229910002804 graphite Inorganic materials 0.000 claims description 17
- 239000010439 graphite Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 15
- 150000005676 cyclic carbonates Chemical class 0.000 claims description 10
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 claims description 9
- 238000010281 constant-current constant-voltage charging Methods 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- 239000000470 constituent Substances 0.000 claims description 5
- 125000004429 atom Chemical group 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 40
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- 230000000996 additive effect Effects 0.000 description 5
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- 159000000002 lithium salts Chemical class 0.000 description 5
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- 239000002184 metal Substances 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
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- 239000002033 PVDF binder Substances 0.000 description 4
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- 239000011889 copper foil Substances 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 4
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- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- SRNYUAJRRLSKFM-UHFFFAOYSA-N [2-oxo-2-(2,2,2-trifluoroethoxy)ethyl]phosphonic acid Chemical compound P(=O)(O)(O)CC(=O)OCC(F)(F)F SRNYUAJRRLSKFM-UHFFFAOYSA-N 0.000 description 3
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- 238000010280 constant potential charging Methods 0.000 description 3
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- 230000001351 cycling effect Effects 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 3
- 229910021469 graphitizable carbon Inorganic materials 0.000 description 3
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
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- 238000007740 vapor deposition Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 2
- NLBSQHGCGGFVJW-UHFFFAOYSA-N 2-carboxyethylphosphonic acid Chemical compound OC(=O)CCP(O)(O)=O NLBSQHGCGGFVJW-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 2
- SWDQZVCRMCJTKA-UHFFFAOYSA-N C(=O)O.P(=O)(O)(O)CC(=O)OCC(F)(F)F Chemical compound C(=O)O.P(=O)(O)(O)CC(=O)OCC(F)(F)F SWDQZVCRMCJTKA-UHFFFAOYSA-N 0.000 description 2
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- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 description 2
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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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
- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M10/00—Secondary cells; Manufacture thereof
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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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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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Abstract
【解決手段】正極、負極、非水電解液およびセパレータを有しており、使用前に4.25Vを超える終止電圧で定電流−定電圧充電が行われるリチウム二次電池であって、非水電解液に、下記一般式(1)で表されるホスホノアセテート類化合物を0.1〜5質量%含有し、かつ1,3−ジオキサンを0.1〜5質量%含有する。
〔前記一般式(1)中、R1、R2およびR3は、それぞれ独立して、ハロゲン原子で置換されていてもよい炭素数1〜12の炭化水素基であり、nは0〜6の整数である。〕
【選択図】なし
Description
トリメチルホスホノフォルメート、メチルジエチルホスホノフォルメート、メチルジプロピルホスホノフォルメート、メチルジブチルホスホノフォルメート、トリエチルホスホノフォルメート、エチルジメチルホスホノフォルメート、エチルジプロピルホスホノフォルメート、エチルジブチルホスホノフォルメート、トリプロピルホスホノフォルメート、プロピルジメチルホスホノフォルメート、プロピルジエチルホスホノフォルメート、プロピルジブチルホスホノフォルメート、トリブチルホスホノフォルメート、ブチルジメチルホスホノフォルメート、ブチルジエチルホスホノフォルメート、ブチルジプロピルホスホノフォルメート、メチルビス(2,2,2−トリフルオロエチル)ホスホノフォルメート、エチルビス(2,2,2−トリフルオロエチル)ホスホノフォルメート、プロピルビス(2,2,2−トリフルオロエチル)ホスホノフォルメート、ブチルビス(2,2,2−トリフルオロエチル)ホスホノフォルメートなど。
トリメチルホスホノアセテート、メチルジエチルホスホノアセテート、メチルジプロピルホスホノアセテート、メチルジブチルホスホノアセテート、トリエチルホスホノアセテート、エチルジメチルホスホノアセテート、エチルジプロピルホスホノアセテート、エチルジブチルホスホノアセテート、トリプロピルホスホノアセテート、プロピルジメチルホスホノアセテート、プロピルジエチルホスホノアセテート、プロピルジブチルホスホノアセテート、トリブチルホスホノアセテート、ブチルジメチルホスホノアセテート、ブチルジエチルホスホノアセテート、ブチルジプロピルホスホノアセテート、メチルビス(2,2,2−トリフルオロエチル)ホスホノアセテート、エチルビス(2,2,2−トリフルオロエチル)ホスホノアセテート、プロピルビス(2,2,2−トリフルオロエチル)ホスホノアセテート、ブチルビス(2,2,2−トリフルオロエチル)ホスホノアセテート、2−プロピニル(ジエチルホスホノ)アセテートなど。
トリメチル−3−ホスホノプロピオネート、メチルジエチル−3−ホスホノプロピオネート、メチルジプロピル−3−ホスホノプロピオネート、メチルジブチル3−ホスホノプロピオネート、トリエチル−3−ホスホノプロピオネート、エチルジメチル−3−ホスホノプロピオネート、エチルジプロピル−3−ホスホノプロピオネート、エチルジブチル3−ホスホノプロピオネート、トリプロピル−3−ホスホノプロピオネート、プロピルジメチル−3−ホスホノプロピオネート、プロピルジエチル−3−ホスホノプロピオネート、プロピルジブチル3−ホスホノプロピオネート、トリブチル−3−ホスホノプロピオネート、ブチルジメチル−3−ホスホノプロピオネート、ブチルジエチル−3−ホスホノプロピオネート、ブチルジプロピル−3−ホスホノプロピオネート、メチルビス(2,2,2−トリフルオロエチル)−3−ホスホノプロピオネート、エチルビス(2,2,2−トリフルオロエチル)−3−ホスホノプロピオネート、プロピルビス(2,2,2−トリフルオロエチル)−3−ホスホノプロピオネート、ブチルビス(2,2,2−トリフルオロエチル)−3−ホスホノプロピオネートなど。
トリメチル−4−ホスホノブチレート、メチルジエチル−4−ホスホノブチレート、メチルジプロピル−4−ホスホノブチレート、メチルジブチル4−ホスホノブチレート、トリエチル−4−ホスホノブチレート、エチルジメチル−4−ホスホノブチレート、エチルジプロピル−4−ホスホノブチレート、エチルジブチル4−ホスホノブチレート、トリプロピル−4−ホスホノブチレート、プロピルジメチル−4−ホスホノブチレート、プロピルジエチル−4−ホスホノブチレート、プロピルジブチル4−ホスホノブチレート、トリブチル−4−ホスホノブチレート、ブチルジメチル−4−ホスホノブチレート、ブチルジエチル−4−ホスホノブチレート、ブチルジプロピル−4−ホスホノブチレートなど。
<正極の作製>
LiCoO2とLi1.0Ni0.5Co0.2Mn0.3O2とを8:2の割合(質量比)で混合した正極活物質100質量部と、バインダであるPVDFを10質量%の濃度で含むNMP溶液20質量部と、導電助剤である人造黒鉛1質量部およびケッチェンブラック1質量部とを、二軸混練機を用いて混練し、更にNMPを加えて粘度を調節して、正極合剤含有ペーストを調製した。
負極活物質である平均粒子径D50%が8μmであるSiO表面を炭素材料で被覆した複合体(複合体における炭素材料の量が10質量%)と、平均粒子径D50%が16μmである黒鉛とを、SiO表面を炭素材料で被覆した複合体の量が3.75質量%となる量で混合した混合物:97.5質量部と、バインダであるSBR:1.5質量部と、増粘剤であるCMC:1質量部とに、水を加えて混合し、負極合剤含有ペーストを調製した。
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)とジエチルカーボネート(DEC)との容積比2:3:1の混合溶媒に、LiPF6を1mol/Lの濃度で溶解させ、更にEDPA、1,3−ジオキサン、VCおよびFECを、それぞれ1質量%となる量で添加して、非水電解液を調製した。
前記帯状の正極を、厚みが16μmの微孔性ポリエチレンセパレータ(空孔率:41%)を介して前記帯状の負極に重ね、渦巻状に巻回した後、扁平状になるように加圧して扁平状巻回構造の電極巻回体とし、この電極巻回体をポリプロピレン製の絶縁テープで固定した。次に、外寸が厚さ4.0mm、幅34mm、高さ50mmのアルミニウム合金製の角形の電池ケースに前記電極巻回体を挿入し、リード体の溶接を行うとともに、アルミニウム合金製の蓋板を電池ケースの開口端部に溶接した。その後、蓋板に設けた注入口から前記非水電解質を注入し、1時間静置した後注入口を封止して、図1に示す構造で、図2に示す外観のリチウム二次電池を得た。
EDPAおよび1,3−ジオキサンの添加量を表1に示すように変更した以外は、実施例1と同様にして非水電解液を調製し、この非水電解液を用いた以外は、実施例1と同様にしてリチウム二次電池を作製した。
EDPAに代えてPDEAを用いた以外は実施例1と同様にして非水電解液を調製し、この非水電解液を用いた以外は実施例1と同様にしてリチウム二次電池を作製した。
LiCoO2とLi0.98Ni0.87Co0.091Mn0.012Al0.012Mg0.012Ba0.0025O2とを8:2の割合(質量比)で混合した正極活物質100質量部と、バインダであるPVDFを10質量%の濃度で含むNMP溶液20質量部と、導電助剤である人造黒鉛1質量部およびケッチェンブラック1質量部とを、二軸混練機を用いて混練し、更にNMPを加えて粘度を調節して、正極合剤含有ペーストを調製した。
比較例1で調製したものと同じ非水電解液を用いた以外は、実施例7と同様にしてリチウム二次電池を作製した。
実施例および比較例の各リチウム二次電池について、1.0Cの電流値で4.35Vまで定電流充電を行い、続いて4.35Vの電圧で定電圧充電を行った。なお、定電流充電と定電圧充電の総充電時間は2.5時間とした。その後、0.2Cの電流値で3.0Vまで放電を行い、初期容量を測定した。
実施例および比較例の各リチウム二次電池について、初期容量測定時と同じ条件で定電流充電および定電圧充電を行い、続いて1.5Cの電流値で3.0Vまで放電を行って放電容量(1.5C放電容量)を求めた。そして、各電池の1.5C放電容量を初期容量で除した値を百分率で表して、容量維持率を求めた。すなわち、この容量維持率が高いほど、電池の負荷特性が優れていることを意味している。
実施例および比較例の各リチウム二次電池(前記の各評価を行った物とは別の電池)について、初期容量測定時と同じ条件で定電流充電および定電圧充電を行い、続いて1.5Cの電流値で3.0Vまで放電を行う一連の操作を1サイクルとして、500サイクルの充放電を繰り返した。その後の各電池について、初期容量測定時と同じ条件で充電および放電を行って、500サイクル経過後の各電池の放電容量を測定し、これを初期容量で除した値を百分率で表して、容量維持率を求めた。この容量維持率が高いほど、電池の充放電サイクル特性が優れているといえる。なお、前記の充放電サイクル特性評価は、室温(25℃)の環境下と、45℃の環境下とで評価を行った。
実施例および比較例の各リチウム二次電池(前記の各評価を行った物とは別の電池)について、初期容量測定時と同じ条件で定電流充電および定電圧充電を行った後に、85℃の環境下で4時間貯蔵し、貯蔵前後での電池の厚み変化(膨れ量)を求めた。
負極活物質を前記の混合物に代えて実施例1で用いたものと同じ黒鉛のみとした以外は実施例1と同様にして負極を作製し、この負極を用いた以外は実施例1と同様にしてリチウム二次電池を作製した。
EDPAに代えてPDEAを用いた以外は実施例1と同様にして非水電解液を調製し、この非水電解液を用いた以外は実施例8と同様にしてリチウム二次電池を作製した。
実施例7で作製したものと同じ正極を用いた以外は、実施例9と同様にしてリチウム二次電池を作製した。
負極活物質を前記の混合物に代えて実施例1で用いたものと同じ黒鉛のみとした以外は実施例1と同様にして負極を作製し、この負極を用いた以外は比較例1と同様にしてリチウム二次電池を作製した。
実施例7で作製したものと同じ正極を用いた以外は、比較例6と同様にしてリチウム二次電池を作製した。
2 負極
3 セパレータ
Claims (7)
- 負極は、SiとOとを構成元素に含む材料(ただし、Siに対するOの原子比xは、0.5≦x≦1.5である)を負極活物質として含有する負極合剤層を、集電体の片面または両面に有するものである請求項1に記載のリチウム二次電池。
- 負極の負極合剤層は、SiとOとを構成元素に含む材料と炭素材料との複合体を含有しており、前記複合体は、前記SiとOとを構成原子に含む材料の表面が、前記炭素材料で被覆されたものである請求項1または2に記載のリチウム二次電池。
- SiとOとを構成元素に含む材料と炭素材料との複合体の表面が、更に炭素材料で被覆されている請求項3に記載のリチウム二次電池。
- 負極の負極合剤層は、負極活物質として黒鉛を含有している請求項1〜4のいずれかに記載のリチウム二次電池。
- ハロゲン置換された環状カーボネートを更に含有する非水電解質を使用した請求項1〜5のいずれかに記載のリチウム二次電池。
- ビニレンカーボネートを更に含有する非水電解質を使用した請求項1〜6のいずれかに記載のリチウム二次電池。
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WO2015111710A1 (ja) * | 2014-01-24 | 2015-07-30 | 日立マクセル株式会社 | 非水二次電池 |
CN103904364B (zh) * | 2014-03-28 | 2017-01-11 | 宁德新能源科技有限公司 | 锂离子二次电池及其电解液 |
KR102352119B1 (ko) * | 2014-03-31 | 2022-01-18 | 다이니폰 인사츠 가부시키가이샤 | 전지용 포장 재료 |
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WO2016068033A1 (ja) * | 2014-10-29 | 2016-05-06 | 日立マクセル株式会社 | リチウムイオン二次電池 |
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JP2017147247A (ja) * | 2017-06-06 | 2017-08-24 | 日本電気株式会社 | 非水電解質二次電池用負極およびこれを用いた非水電解質二次電池 |
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US20130344381A1 (en) | 2013-12-26 |
CN103515666A (zh) | 2014-01-15 |
KR20140000167A (ko) | 2014-01-02 |
CN103515666B (zh) | 2017-03-01 |
US9005824B2 (en) | 2015-04-14 |
JP6279233B2 (ja) | 2018-02-14 |
KR102044438B1 (ko) | 2019-11-13 |
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