JPWO2013146300A1 - 非水電解質二次電池用負極活物質粒子粉末及びその製造方法、並びに非水電解質二次電池 - Google Patents
非水電解質二次電池用負極活物質粒子粉末及びその製造方法、並びに非水電解質二次電池 Download PDFInfo
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- JPWO2013146300A1 JPWO2013146300A1 JP2014507663A JP2014507663A JPWO2013146300A1 JP WO2013146300 A1 JPWO2013146300 A1 JP WO2013146300A1 JP 2014507663 A JP2014507663 A JP 2014507663A JP 2014507663 A JP2014507663 A JP 2014507663A JP WO2013146300 A1 JPWO2013146300 A1 JP WO2013146300A1
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- negative electrode
- active material
- secondary battery
- electrode active
- electrolyte secondary
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Classifications
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
-
- 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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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/137—Electrodes based on electro-active polymers
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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Abstract
Description
負極活物質の体積膨張を抑制するため、樹脂で活物質を覆うことが有効であると考え、Li活性な金属粒子を熱硬化性樹脂で被覆すること、被覆した樹脂をグラファイト化することで活物質に導電性を持たせることによって、負極活物質として特性向上することができた。体積膨張を抑制する理由として、金属粒子の周りに樹脂及び/又はその炭化物が存在することで、金属活物質のLi吸蔵による膨張に伴う体積変化を吸収することができることによるものと推定している。
電極密度(g/cm3)=(打ち抜きシート重量―アルミ箔重量)
/(打ち抜きシート面積×(打ち抜きシート厚さーアルミ箔の厚さ))
高:1.3g/cm3以上
低:1.3g/cm3未満
本発明における実施例で得られた負極活物質を用い、活物質:アセチレンブラック:PVdF=9:1:1(wt%)になるよう調整して、ギャップ150μmのドクターブレードで電極スラリーをAl箔集電体上に塗布した。シート乾燥後、3t/cm2に加圧しシート表面を目視で観察し、下記2段階で評価した。
良:シート表面に塗布ムラが確認されない
悪:シート表面に塗布ムラが確認される
本発明における実施例で得られた負極活物質を用い、活物質:アセチレンブラック:PVdF=9:1:1(wt%)になるよう調整して、Cu箔上に塗工し、110℃で3時間乾燥した。このシートを16mmφに打ち抜いた後、1t/cm2で圧着し、集電体上の電極膜厚を20μmとしたものを負極に用いた。
正極は16mmφに打ち抜いた金属リチウムとし、電解液は1mol/lのLiPF6を溶解したECとDMCを体積比で1:2で混合した溶液を用いてCR2032型コインセルを作製した。
1リットルフラスコ内にフェノール67.8g、ホルマリン53.9g、粒子表面がエポキシ基を有するシランカップリング剤で処理されている上記粉末200g、アンモニア水24.2g及び水6gを仕込み、撹拌しながら30分間で85℃に上昇させた後、同温度で120分間反応・硬化させることにより、シリコン粒子粉末とフェノール樹脂とからなる複合体の生成を行った。
次に、フラスコ内の内容物を30℃に冷却し、1.5リットルの水を添加した後、上澄み液を除去し、さらに下層の沈殿物を水洗し、80℃に設定した乾燥機中で12時間乾燥させ、平均粒径(D50)が15.2μmであるシリコン粒子粉末とフェノール樹脂とからなる球状の複合体の粒子を得た。
図1、2に示すように金属活物質が樹脂に内包され球状であり、且つ固められていて密度の高い粒子であることがわかる。
上記実施例1で得られた複合体粒子を還元性雰囲気中(N2)、1000℃で2時間熱処理を行って、シリコン粉末と炭素とからなる負極活物質を得た。得られた負極活物質粒子粉末の諸特性を表1に示す。
前記実施例2に対して種々条件を変更し、300〜1200℃の間の温度で熱処理を行って、負極活物質粒子粉末を得た。
Claims (8)
- 金属粒子と熱硬化性樹脂との複合粒子粉末からなる非水電解質二次電池用負極活物質であって、前記複合粒子粉末の平均粒径が5〜100μmであることを特徴とする非水電解質二次電池用負極活物質。
- 熱硬化性樹脂の含有量が5.0〜30wt%である請求項1記載の非水電解質二次電池用負極活物質。
- 金属粒子と熱硬化性樹脂の炭化物との複合粒子粉末からなる非水電解質二次電池用負極活物質であって、前記複合粒子粉末の平均粒径が5〜100μmであることを特徴とする非水電解質二次電池用負極活物質。
- 炭化物の含有量が0.1〜20wt%である請求項3記載の非水電解質二次電池用負極活物質。
- 熱硬化性樹脂が熱硬化性フェノール樹脂又は熱硬化性エポキシ樹脂からなる請求項1〜4のいずれかに記載の非水電解質二次電池用負極活物質。
- 非水電解質二次電池用負極活物質の粒子内部及び粒子表面に、結晶性炭素又はカーボンナノチューブから選ばれる1種または2種類以上の炭素を含有する請求項1〜5のいずれかに記載の非水電解質二次電池用負極活物質。
- 金属粒子と熱硬化性フェノール樹脂又は熱硬化性エポキシ樹脂とを造粒して複合体とした後、当該複合体を還元性雰囲気中で300〜1200℃で加熱処理する請求項3記載の負極活物質の製造方法。
- 負極材として請求項1〜6のいずれかに記載の非水電解質二次電池用負極活物質を用いることを特徴とするリチウムイオン二次電池。
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JP2015118871A (ja) * | 2013-12-19 | 2015-06-25 | 凸版印刷株式会社 | 非水電解質二次電池用負極、及び非水電解質二次電池 |
KR102237829B1 (ko) * | 2013-12-30 | 2021-04-08 | 삼성전자주식회사 | 리튬 이차 전지용 음극재, 그 제조방법, 이를 음극으로 포함하는 리튬 이차 전지 |
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CN106469814B (zh) * | 2016-04-14 | 2019-11-29 | 山东圣泉新能源科技有限公司 | 一种包覆剂、负极材料、锂离子电池及其制备方法 |
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