JP2020518962A - 負極活物質、前記負極活物質を含む負極、前記負極を含む二次電池及び前記負極活物質の製造方法 - Google Patents
負極活物質、前記負極活物質を含む負極、前記負極を含む二次電池及び前記負極活物質の製造方法 Download PDFInfo
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Abstract
Description
本出願は、2017年5月4日付出願された韓国特許出願第10−2017−0057049号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示された全ての内容は本明細書の一部として含まれる。
製造例1:ケイ素系化合物の製造
SiO粉末20g及び金属リチウムパウダー2gを混合した後、チャンバの反応容器中に収納し、引き続き、前記チャンバの温度を800℃に昇温した。このとき、不活性ガスはArを用いた。以後、2時間熱処理した後、チャンバ温度を常温に減温し、反応容器中の生成物を捕集した。捕集された生成物をHClを用いて酸処理した。以後、酸処理された生成物を平均粒径(D50)が5μmとなるようにミーリングし、ケイ素系化合物を製造した。XRDで測定した結果、前記ケイ素系化合物は、内部に金属シリケートであるLi2SiO3及びLi2Si2O3を含み、リチウムは、前記ケイ素系化合物100重量部に対して総5重量部で含まれていることを確認した。
チャンバ内に製造例1のケイ素系化合物を配置させた後、アルミニウムアセトネートをソースとした化学気相蒸着法を行った。このとき、チャンバ内の温度は450℃であり、化学気相蒸着法は10SCCM、10−1torrで0.5分間進められた。これを介してケイ素系化合物上に結晶質炭素層を形成させ、負極活物質を製造した。
チャンバ内に製造例1のケイ素系化合物を配置させた後、アルミニウムアセトネートをソースとした化学気相蒸着法を行った。このとき、チャンバ内の温度は450℃であり、化学気相蒸着法は10SCCM、10−1torrで10分間進められた。これを介してケイ素系化合物上に結晶質炭素層を形成させ、負極活物質を製造した。
チャンバ内に製造例1のケイ素系化合物を配置させた後、アルミニウムアセトネートをソースとした化学気相蒸着法を行った。このとき、チャンバ内の温度は450℃であり、化学気相蒸着法は10SCCM、10−1torrで5分間進められた。これを介してケイ素系化合物上に結晶質炭素層を形成させ、負極活物質を製造した。
チャンバ内に製造例1のケイ素系化合物を配置させた後、メタンソースを用いて化学気相蒸着法を行った。このとき、チャンバ内の温度は900℃であり、化学気相蒸着法は20分間10−1torrで進められた。これを介してケイ素系化合物上に非晶質炭素層を形成させ、負極活物質を製造した。
実施例1から3及び比較例1の負極活物質をそれぞれ用いて、実施例4から6及び比較例2の負極スラリーを製造した。具体的に、実施例1から3及び比較例1それぞれの負極活物質、天然黒鉛、平均粒径(D50)が65nmであるカーボンブラック、CMC、スチレンブタジエンゴム(SBR)を重量比9.6:86.2:1.0:1.7:1.5で溶媒である蒸溜水に添加及び混合し、混合物固形分45%の負極スラリーを製造した。
実施例4から6及び比較例2の負極スラリーそれぞれに対し、次のような方法で水分安定性を評価した後、表2に示した。実施例4から6及び比較例2の負極スラリーそれぞれを密閉されたセルに投入した後、密閉されたセルに連結された圧力測定器でガス発生の時点を測定した。
実施例4から6及び比較例2の負極スラリーそれぞれを、厚さが20μmの負極集電体である銅(Cu)金属薄膜に160mg/25cm2のローディングで塗布、乾燥した。このとき、循環される空気の温度は60℃であった。次いで、前記スラリーが塗布、乾燥された負極集電体を圧延(roll press)し、130℃の真空オーブンで8時間乾燥させて負極を製造した。
実施例7から9及び比較例3の二次電池それぞれに対し、次のような方法で容量維持率を評価した後、表3に示した。
充電条件:CC(定電流)/CV(定電圧)(5mV/0.005C current cut−off)
放電条件:CC(定電流)条件1.0V
容量維持率は、それぞれ次のような計算によって導き出された。
容量維持率(%)=(50回放電容量/1回1.0V放電容量)×100
Claims (15)
- SiOx(0.5<x<1.3)を含むケイ素系化合物を準備する段階;及び
有機金属化合物をソースとした化学気相蒸着法を介して前記ケイ素系化合物上に結晶質炭素コーティング層を形成する段階を含み、
前記有機金属化合物は、アルミニウムアセチルアセトネート、アルミニウムエトキシド、アルミニウムフェノキシド、アルミニウムアセテート及びアルミニウムトリブトキシドからなる群より選択される少なくとも何れか一つである、負極活物質の製造方法。 - 前記ケイ素系化合物を準備する段階は、
SiOx1(0<x1<2)を、金属を含む金属性パウダーまたは金属性ガスと反応させることである、請求項1に記載の負極活物質の製造方法。 - 前記金属は、Li、Mg、Ti及びCaからなる群より選択される少なくとも何れか一つである、請求項2に記載の負極活物質の製造方法。
- 前記化学気相蒸着法は、
前記有機金属化合物を気化させること、及び
前記気化された有機金属化合物を前記ケイ素系化合物が配置されたチャンバ内に流入させることを含み、
前記有機金属化合物の流入速度は1SCCMから50SCCMである、請求項1に記載の負極活物質の製造方法。 - 前記チャンバ内の温度は300℃から1000℃であり、
前記化学気相蒸着法は0.5分から1時間行われる、請求項4に記載の負極活物質の製造方法。 - SiOx(0.5<x<1.3)を含むケイ素系化合物;及び
前記ケイ素系化合物上に配置された結晶質炭素コーティング層を含み、
前記結晶質炭素コーティング層はアルミニウムを含む負極活物質。 - 前記アルミニウムは、前記結晶質炭素コーティング層100重量部に対して1重量部から10重量部で含まれる、請求項6に記載の負極活物質。
- 前記ケイ素系化合物は金属シリケートをさらに含み、
前記金属シリケートは、Li2Si2O5、Li3SiO3、Li4SiO4、Mg2SiO4、MgSiO3、Ca2SiO4、CaSiO3、及びTiSiO4からなる群より選択される少なくとも何れか一つを含む、請求項6に記載の負極活物質。 - 前記金属シリケートの金属は、前記SiOx(0.5<x<1.3)100重量部に対して1重量部から30重量部で含まれる、請求項8に記載の負極活物質。
- 前記結晶質炭素コーティング層のラマンスペクトルのD/G比率が0超過1未満で、2D/G比率が0超過1未満である、請求項6に記載の負極活物質。
- 前記結晶質炭素コーティング層の厚さは0.01μmから1μmである、請求項6に記載の負極活物質。
- 前記ケイ素系化合物の平均粒径(D50)は0.5μmから10μmである、請求項6に記載の負極活物質。
- 請求項6に記載の負極活物質を含む負極。
- 黒鉛系粒子をさらに含む、請求項13に記載の負極。
- 請求項14に記載の負極;
正極;
前記正極と前記負極の間に介在された分離膜;及び
電解質を含む二次電池。
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KR10-2017-0057049 | 2017-05-04 | ||
PCT/KR2018/003627 WO2018203599A1 (ko) | 2017-05-04 | 2018-03-27 | 음극 활물질, 상기 음극 활물질을 포함하는 음극, 상기 음극을 포함하는 이차 전지 및 상기 음극 활물질의 제조 방법 |
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US11588150B2 (en) * | 2019-05-20 | 2023-02-21 | Nanograf Corporation | Anode active material including low-defect turbostratic carbon |
EP3993103A4 (en) * | 2019-06-28 | 2023-01-25 | SANYO Electric Co., Ltd. | NEGATIVE ELECTRODE ACTIVE MATERIAL FOR SECONDARY BATTERIES, AND SECONDARY BATTERY |
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CN111342030B (zh) * | 2020-03-28 | 2022-03-15 | 兰溪致德新能源材料有限公司 | 一种多元复合高首效锂电池负极材料及其制备方法 |
KR102286227B1 (ko) * | 2020-05-21 | 2021-08-06 | 에스케이이노베이션 주식회사 | 리튬이 도핑된 규소계 산화물 음극 활물질, 이의 제조방법, 이를 포함하는 음극 및 이차전지 |
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EP3598540A1 (en) | 2020-01-22 |
CN118039840A (zh) | 2024-05-14 |
EP3598540A4 (en) | 2020-05-06 |
JP7045556B2 (ja) | 2022-04-01 |
US11437611B2 (en) | 2022-09-06 |
KR102164252B1 (ko) | 2020-10-12 |
WO2018203599A1 (ko) | 2018-11-08 |
KR20180122871A (ko) | 2018-11-14 |
CN110612625A (zh) | 2019-12-24 |
EP3598540B1 (en) | 2020-12-23 |
US20210151742A1 (en) | 2021-05-20 |
PL3598540T3 (pl) | 2021-06-28 |
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