JPWO2016170756A1 - 非水電解質二次電池 - Google Patents
非水電解質二次電池 Download PDFInfo
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- JPWO2016170756A1 JPWO2016170756A1 JP2017513959A JP2017513959A JPWO2016170756A1 JP WO2016170756 A1 JPWO2016170756 A1 JP WO2016170756A1 JP 2017513959 A JP2017513959 A JP 2017513959A JP 2017513959 A JP2017513959 A JP 2017513959A JP WO2016170756 A1 JPWO2016170756 A1 JP WO2016170756A1
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- Prior art keywords
- positive electrode
- negative electrode
- oxide
- lithium
- secondary battery
- Prior art date
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- AWROWLLGXAQBQF-UHFFFAOYSA-N dilithium hydrogen phosphite Chemical compound [Li+].[Li+].OP([O-])[O-] AWROWLLGXAQBQF-UHFFFAOYSA-N 0.000 description 1
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- BRFMYUCUGXFMIO-UHFFFAOYSA-N phosphono dihydrogen phosphate phosphoric acid Chemical compound OP(O)(O)=O.OP(O)(=O)OP(O)(O)=O BRFMYUCUGXFMIO-UHFFFAOYSA-N 0.000 description 1
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- 239000011163 secondary particle Substances 0.000 description 1
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- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- IAHFWCOBPZCAEA-UHFFFAOYSA-N succinonitrile Chemical compound N#CCCC#N IAHFWCOBPZCAEA-UHFFFAOYSA-N 0.000 description 1
- 125000001174 sulfone group Chemical group 0.000 description 1
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- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
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- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 150000003658 tungsten compounds Chemical class 0.000 description 1
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Abstract
Description
正極は、金属箔等の正極集電体と、正極集電体上に形成された正極合材層とで構成される。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。正極合材層には、リチウム遷移金属酸化物と、リン酸化合物とが含まれ、さらに導電材及び結着材が含まれることが好適である。正極合材層中にリン酸化合物が含まれることで、充電時においてリチウム遷移金属酸化物の表面に良質な保護被膜が形成され、電池の充放電サイクル時や保存時のガス発生が抑制されると考えられる。正極は、例えば正極集電体上にリチウム遷移金属酸化物、リン酸化合物、導電材、及び結着材等を含む正極合材スラリーを塗布し、塗膜を乾燥させた後、圧延して正極合材層を集電体の両面に形成することにより作製できる。
くとも1種)で表されるオリビン構造を有するものであってもよい。正極活物質には、リチウム遷移金属酸化物を1種単独で用いてもよいし、複数種を混合して用いてもよい。
らの樹脂と、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)等が併用されてもよい。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。
負極は、金属箔等からなる負極集電体と、当該集電体上に形成された負極合材層とで構成される。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、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。負極集電体は、銅箔、ニッケル箔、ステンレス箔等であってもよいが、負極活物質として4−6族酸化物を用いる場合はアルミニウム箔が好ましい。負極合材層は、負極活物質に加えて、結着材を含むことが好適であり、負極活物質として4−6族酸化物を用いる場合はさらに導電材を含むことが好適である。負極は、例えば負極集電体上に負極活物質、結着材等を含む負極合材スラリーを塗布し、塗膜を乾燥させた後、圧延して負極合材層を集電体の両面に形成することにより作製できる。
セパレータは、イオン透過性及び絶縁性を有する多孔質膜であって、セルロースを主成分として構成されるセルロースセパレータである。セルロースセパレータは、上記のように機械的強度、通気性、耐熱性等に優れるが、セルロース分子が水酸基を多く含むため、吸湿性を有する。セルロースセパレータは、例えばセルロース繊維を主成分とする不織布である。ここで、セルロース(セルロース繊維)を主成分とするとは、セパレータの構成材料に対するセルロースの質量比が最も高いことを意味し、好ましくはセパレータの総質量に対してセルロースが80質量%以上含まれる。セルロースセパレータは、セルロース繊維以外の有機繊維、例えばアラミド繊維、ポリオレフィン繊維、ポリアミド繊維、ポリイミド繊維等を含んでいてもよく、シリカ、アルミナ等の微粒子を含んでいてもよい。セルロースセパレータは、実質的にセルロースのみから構成されていてもよい。
空隙率(%) = (1−見掛け密度/真密度)×100・・・式(1)
非水電解質には、フッ素(F)を含有する含フッ素非水電解質が用いられる。含フッ素非水電解質は、例えば非水溶媒と、非水溶媒に溶解したフッ素含有電解質塩(溶質)とを含む。非水電解質は、液体電解質(非水電解液)に限定されず、ゲル状ポリマー等を用いた固体電解質であってもよい。非水溶媒は、溶媒分子の水素の少なくとも一部がフッ素等のハロゲン原子で置換されたハロゲン置換体であってもよい。
[正極活物質の作製]
共沈により得られた[Ni0.50Co0.20Mn0.30](OH)2で表される水酸化物を500℃で焼成して、ニッケルコバルトマンガン複合酸化物を得た。次に、炭酸リチウムと、上記ニッケルコバルトマンガン複合酸化物と、酸化タングステン(WO3)とを、Liと、Ni、Co、及びMnの総量と、WO3中のWとのモル比が1.2:1:0.005になるように、石川式らいかい乳鉢にて混合した。この混合物を空気雰囲気中にて900℃で20時間熱処理し、粉砕することにより、タングステンが固溶したLi1.07[Ni0.465Co0.186Mn0.279W0.005]O2で表されるリチウム遷移金属酸化物を得た。得られた複合酸化物の粉末を走査型電子顕微鏡(SEM)で観察して、酸化タングステンの未反応物が残っていないことを確認した。
上記正極活物質と、活物質に対して2質量%のリン酸リチウム(Li3PO4)とを混合した。当該混合物と、アセチレンブラックと、ポリフッ化ビニリデンとを、93.5:5:1.5の質量比で混合し、N−メチル−2−ピロリドンを適量加えた後、これを混練して正極合材スラリーを調製した。当該正極合材スラリーを、アルミニウム箔からなる正極集電体の両面に塗布し、塗膜を乾燥させた後、圧延ローラーにより圧延し、さらにアルミニウム製の集電タブを取り付けることにより、正極集電体の両面に正極合剤層が形成された正極を作製した。得られた正極をSEMで観察したところ、平均粒径が150nmの酸化タングステン粒子がリチウム遷移金属酸化物の粒子表面に付着していることが確認された。
市販試薬であるLiOH・H2OとTiO2の原料粉末を、LiとTiとのモル比が化学量論比よりもややLi過剰となるように秤量し、これらを乳鉢で混合した。原料のTiO2には、アナターゼ型の結晶構造を有するものを用いた。混合した原料粉末をAl2O3製のるつぼに入れ、大気雰囲気中850℃で12時間熱処理し、熱処理した材料を乳鉢で粉砕して、チタン酸リチウム(Li4Ti5O12)の粗粉末を得た。得られたLi4Ti5O12の粗粉末の粉末X線回折測定を行ったところ、空間群がFd3mに帰属されるスピネル型構造からなる単相の回折パターンが得られた。Li4Ti5O12の粗粉末をジェットミル粉砕及び分級して、Dv50が0.7μmのLi4Ti5O12粉末を得た。このLi4Ti5O12粉末を負極活物質として用いる。Li4Ti5O12粉末のBET比表面積を比表面積測定装置(島津製作所製、トライスターII 3020)を用いて測定したところ、6.8m2/gであった。
上記負極活物質と、カーボンブラックと、ポリフッ化ビニリデンとを、100:7:3の質量比で混合し、N−メチル−2−ピロリドンを適量加えた後、これを混練して負極合剤スラリーを調製した。当該負極合剤スラリーを、アルミニウム箔からなる負極集電体の両面に塗布し、塗膜を乾燥させた後、圧延ローラーにより圧延し、さらにニッケル製の集電タブを取り付けることにより、負極集電体の両面に負極合剤層が形成された負極を作製した。
プロピレンカーボネート(PC)と、エチルメチルカーボネート(EMC)と、ジメチルカーボネート(DMC)とを、25:35:40の体積比で混合した混合溶媒に、LiPF6を1.2モル/リットルの割合で溶解させて、含フッ素非水電解質を調製した。
セルロースセパレータを介して、上記正極及び上記負極渦巻き状に巻回し、105℃150分の条件で真空乾燥して巻回型の電極体を作製した。セルロースセパレータは、セルロース繊維から構成される不織布であって、厚み20μm、空隙率75%、通気度8秒/100ccであった。アルゴン雰囲気下のグローブボックス中にて、電極体及び非水電解質をアルミニウムラミネートシートで構成される外装体内に封入することにより、電池A1を作製した。電池A1の設計容量は15.6mAhであった。
正極の作製において、Li3PO4を混合しなかったこと以外は、上記実験例1と同様にして電池A2を作製した。
電池A1、A2について、以下の条件で20サイクルの充放電を行い、3日間保存した後、ガス発生量を求めた。
1サイクル目の充放電条件:25℃の温度条件下において、0.22It(3.5mA)の充電電流で電池電圧が2.65Vまで定電流充電を行い、次に0.22It(3.5mA)の放電電流で1.5Vまで定電流放電した。
上記20サイクルの充放電後に、25℃の温度条件において、2.65Vまで定電流充電を行った。続いて、60℃の温度条件で3日間静置し、その後25℃の温度条件において放電させた。
充放電前及び上記保存試験後の各電池について、アルキメデス法に基づき、大気中における電池質量と水中における電池質量の差を測定し、電池にかかる浮力(体積)を算出した。充放電試験前の浮力と保存試験後の浮力の差をガス発生量とした。
電池の作製において、ポリプロピレン(PP)/ポリエチレン(PE)/ポリプロピレン(PP)の三層構造を有する微多孔膜をセパレータに用いたこと以外は、実験例1と同様にして電池B1を作製し、上記保存試験後のガス発生量を求めた。
正極の作製において、Li3PO4を混合しなかったこと以外は、上記参考例1と同様にして電池B2を作製し、上記保存試験後のガス発生量を求めた。
Claims (6)
- 正極集電体上に正極合材層が形成された正極と、負極集電体上に負極合材層が形成された負極と、セルロースを主成分として構成されるセパレータと、含フッ素非水電解質とを備える非水電解質二次電池であって、
前記正極合材層には、リチウム遷移金属酸化物と、リン酸化合物とが含まれる、非水電解質二次電池。 - 前記負極合材層には、周期表の4族元素、5族元素、及び6族元素から選択される少なくとも1種を含有する4−6族酸化物が含まれる、請求項1に記載の非水電解質二次電池。
- 前記4−6族酸化物は、チタン酸リチウムである、請求項2に記載の非水電解質二次電池。
- 前記リン酸化合物は、リン酸リチウムである、請求項1〜3のいずれか1項に記載の非水電解質二次電池。
- 前記リチウム遷移金属酸化物には、タングステンが固溶しており、且つ当該金属酸化物の表面には、酸化タングステンが付着している、請求項1〜4のいずれか1項に記載の非水電解質二次電池。
- 前記酸化タングステンは、WO3である、請求項5に記載の非水電解質二次電池。
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