JP2023513429A - 二次電池用正極活物質およびこれを含むリチウム二次電池 - Google Patents
二次電池用正極活物質およびこれを含むリチウム二次電池 Download PDFInfo
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- JP2023513429A JP2023513429A JP2022544179A JP2022544179A JP2023513429A JP 2023513429 A JP2023513429 A JP 2023513429A JP 2022544179 A JP2022544179 A JP 2022544179A JP 2022544179 A JP2022544179 A JP 2022544179A JP 2023513429 A JP2023513429 A JP 2023513429A
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- positive electrode
- lithium
- active material
- secondary battery
- transition metal
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 101
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 69
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000002245 particle Substances 0.000 claims abstract description 68
- 239000002131 composite material Substances 0.000 claims abstract description 43
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 43
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 36
- 239000013078 crystal Substances 0.000 claims abstract description 23
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- 239000002184 metal Substances 0.000 claims abstract description 18
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 8
- 239000010941 cobalt Substances 0.000 claims abstract description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000002739 metals Chemical class 0.000 claims abstract description 6
- -1 nickel cations Chemical class 0.000 claims description 19
- 239000011572 manganese Substances 0.000 claims description 18
- 239000006182 cathode active material Substances 0.000 claims description 15
- 238000004627 transmission electron microscopy Methods 0.000 claims description 14
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- 239000000126 substance Substances 0.000 claims description 11
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- 229910052719 titanium Inorganic materials 0.000 claims description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
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- 238000002156 mixing Methods 0.000 claims description 4
- 239000011149 active material Substances 0.000 claims description 3
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- 229910052720 vanadium Inorganic materials 0.000 claims description 2
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
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- 239000006234 thermal black Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- 239000002733 tin-carbon composite material Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本発明の二次電池用正極活物質は、ニッケル、コバルトおよびマンガンを含み、リチウム以外の金属のうちニッケルを60モル%以上含有するリチウム複合遷移金属酸化物であり、平均粒径(D50)が1~10μmである単粒子であり、前記リチウム複合遷移金属酸化物の粒子の表面から粒子の中心方向に100nmの領域は、Fd3m空間群およびFm3m空間群の結晶構造を含み、前記リチウム複合遷移金属酸化物の粒子に対して、TEM(Transmission Electron Microscopy,透過型電子顕微鏡法)を用いて、粒子表面部の断面イメージを得た時に、前記Fd3m空間群の結晶構造およびFm3m空間群の結晶構造が占める各部分の最大直線長さの比率である相の比率(phase ratio)Fd3m/Fm3mが0.2~0.7である。
LiaNi1-b-c-dCobMncQdO2+δ
本発明の他の一実施形態によると、前記のように製造された正極活物質を含む二次電池用正極およびリチウム二次電池を提供する。
正極活物質前駆体Ni0.85Co0.05Mn0.10(OH)2にLi/Metal(Ni、Co、Mn)モル比が1.15になるようにリチウムソースLiOHを入れて混合し、B2O3 1wt%、K2CO3 1wt%を入れて混合した。一次熱処理のために混合した粉末をアルミナるつぼに投入した。次に、850℃、酸素雰囲気下で20時間焼成してリチウム複合遷移金属酸化物を製造した。以降、粉砕および水洗、乾燥工程を経た粉末にH3BO3 0.1wt%を混合し、300℃Air雰囲気下で二次熱処理して、単粒子形状を有する正極活物質を得た。
Li/Metal(Ni、Co、Mn)モル比が1.11になるようにし、一次熱処理温度を830℃にした以外は、実施例1と同様に実施して正極活物質を製造した。
Li/Metal(Ni、Co、Mn)モル比が1.18になるようにし、一次熱処理温度を870℃にした以外は、実施例1と同様に実施して正極活物質を製造した。
Li/Metal(Ni、Co、Mn)モル比が1.18になるようにし、一次熱処理温度を890℃にした以外は、実施例1と同様に実施して正極活物質を製造した。
Li/Metal(Ni、Co、Mn)モル比が1.05になるようにし、一次熱処理温度を950℃にした以外は、実施例1と同様に実施して正極活物質を製造した。
Li/Metal(Ni、Co、Mn)モル比が1.02になるようにし、一次熱処理温度を780℃にした以外は、実施例1と同様に実施して正極活物質を製造した。
Li/Metal(Ni、Co、Mn)モル比が1.02になるようにし、一次熱処理温度を780℃にし、B2O3 1wt%、K2CO3 1wt%を混合しない以外は、実施例1と同様に実施して正極活物質を製造した。
実施例1~4および比較例1~3で製造された正極活物質をTEMを用いて表面の相分析を実施し、各相が占める部分の最大直線長さを測定した後、その比率を計算して、表面から粒子の中心方向にそれぞれ100nmの領域でのFd3m空間群およびFm3m空間群の相の比率(phase ratio)Fd3m/Fm3mを測定した。その結果を下記表1に示し、実施例2に対するTEM写真を図1に示した。
前記実施例1~4、比較例1で製造されたそれぞれの正極活物質、カーボンブラック導電材およびPVDFバインダーをN‐メチルピロリドン溶媒の中で重量比96:2:2の比率で混合して正極合材(粘度:5000mPa・s)を製造し、これをアルミニウム集電体の一面に塗布してから130℃で乾燥した後、圧延して正極を製造した。
前記実施例1~4、比較例1~2で製造されたそれぞれの正極活物質を適用して実験例2のように製造された各リチウム二次電池ハーフセル(half‐cell)に対して、25℃、SOC10%に1.0Cの放電をさせた時の直流抵抗を測定した。抵抗の計算は、当該SOCで1.0Cで10秒間放電させた時の電圧降下と印加された電流値を基準として行った。下記表3にその結果として計算された抵抗値を示した。
前記実施例1~4および比較例1~3で製造されたそれぞれの正極活物質を使用して、リチウム二次電池フルセル(full cell)を製造した。実験例2でのように製造し、この際、負極は、負極活物質として黒鉛(graphite)、カーボンブラック導電材およびPVDFバインダーをN‐メチルピロリドン溶媒の中で重量比96:2:2の比率で混合して負極合材を製造し、これを銅集電体の一面に塗布してから130℃で乾燥した後、圧延して製造した。
抵抗増加率=(100サイクルでの放電抵抗/1サイクルでの放電抵抗)×100
前記実施例1~4および比較例1~3で製造されたそれぞれの正極活物質を使用して、実験例2のようにリチウム二次電池ハーフセル(half cell)を製造した。前記のように製造された各リチウム二次電池ハーフセル(half cell)に対して、4.7Vまで充電させた後、CVモードで120時間維持した。この時に発生した電流(current)値を積分し時間で除して平均電流値を計算し、その結果を下記表5に示した。
Claims (9)
- ニッケル、コバルトおよびマンガンを含み、リチウム以外の金属のうちニッケルを60モル%以上含有するリチウム複合遷移金属酸化物であり、
平均粒径(D50)が1~10μmである単粒子であり、
前記リチウム複合遷移金属酸化物の粒子の表面から粒子の中心方向に100nmの領域は、Fd3m空間群およびFm3m空間群の結晶構造を含み、
前記リチウム複合遷移金属酸化物の粒子に対して、TEM(透過型電子顕微鏡法)を用いて粒子表面部の断面イメージを得た時に、前記Fd3m空間群の結晶構造およびFm3m空間群の結晶構造が占める各部分の最大直線長さの比率である相の比率Fd3m/Fm3mが0.2~0.7である、二次電池用正極活物質。 - 前記相の比率Fd3m/Fm3mが0.3~0.6である、請求項1に記載の二次電池用正極活物質。
- 平均粒径(D50)が2~7μmである単粒子形状である、請求項1に記載の二次電池用正極活物質。
- 前記リチウム複合遷移金属酸化物の構造内のリチウム層でのニッケルカチオンのカチオンミキシングの比率が1.5%以下である、請求項1に記載の二次電池用正極活物質。
- 前記リチウム複合遷移金属酸化物の構造内のリチウム層でのニッケルカチオンのカチオンミキシングの比率が1.0%以下である、請求項4に記載の二次電池用正極活物質。
- 前記リチウム複合遷移金属酸化物は、リチウム以外の金属(M)に対するリチウムのモル比(Li/M)が1.1~1.2である、請求項1に記載の二次電池用正極活物質。
- 前記リチウム複合遷移金属酸化物は、下記化学式1で表され、
[化学式1]
LiaNi1-b-c-dCobMncQdO2+δ
前記化学式1中、Qは、Al、Mg、V、TiおよびZrからなる群から選択されるいずれか一つ以上の元素であり、1.0≦a≦1.2、0<b≦0.4、0<c≦0.3、0≦d≦0.1、0<b+c+d≦0.4、-0.1≦δ≦1.0である、請求項1に記載の二次電池用正極活物質。 - 請求項1から請求項7のいずれか一項に記載の正極活物質を含む二次電池用正極。
- 請求項8に記載の正極を含むリチウム二次電池。
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