JP6686652B2 - 炭素被覆Si含有負極活物質の製造方法 - Google Patents
炭素被覆Si含有負極活物質の製造方法 Download PDFInfo
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- JP6686652B2 JP6686652B2 JP2016080336A JP2016080336A JP6686652B2 JP 6686652 B2 JP6686652 B2 JP 6686652B2 JP 2016080336 A JP2016080336 A JP 2016080336A JP 2016080336 A JP2016080336 A JP 2016080336A JP 6686652 B2 JP6686652 B2 JP 6686652B2
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- 229910052799 carbon Inorganic materials 0.000 title claims description 123
- 239000007773 negative electrode material Substances 0.000 title claims description 123
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
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- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 4
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- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
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- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- YRPQTVNCCVPGFA-FPLPWBNLSA-N palmitoleamide Chemical compound CCCCCC\C=C/CCCCCCCC(N)=O YRPQTVNCCVPGFA-FPLPWBNLSA-N 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- KHUXNRRPPZOJPT-UHFFFAOYSA-N phenoxy radical Chemical group O=C1C=C[CH]C=C1 KHUXNRRPPZOJPT-UHFFFAOYSA-N 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
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- 229920000767 polyaniline Polymers 0.000 description 1
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- 229920001282 polysaccharide Polymers 0.000 description 1
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- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
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- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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- 239000003586 protic polar solvent Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
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- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 229940045870 sodium palmitate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229940080350 sodium stearate Drugs 0.000 description 1
- DDMGAAYEUNWXSI-XVSDJDOKSA-M sodium;(5z,8z,11z,14z)-icosa-5,8,11,14-tetraenoate Chemical compound [Na+].CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC([O-])=O DDMGAAYEUNWXSI-XVSDJDOKSA-M 0.000 description 1
- WYPBVHPKMJYUEO-NBTZWHCOSA-M sodium;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Na+].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O WYPBVHPKMJYUEO-NBTZWHCOSA-M 0.000 description 1
- RUMMJKMQGVFYDJ-CMBBICFISA-M sodium;(e)-4-hexadecoxy-4-oxobut-2-enoate Chemical compound [Na+].CCCCCCCCCCCCCCCCOC(=O)\C=C\C([O-])=O RUMMJKMQGVFYDJ-CMBBICFISA-M 0.000 description 1
- GGXKEBACDBNFAF-UHFFFAOYSA-M sodium;hexadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCC([O-])=O GGXKEBACDBNFAF-UHFFFAOYSA-M 0.000 description 1
- MRQYKJNZWPCFNB-UHFFFAOYSA-M sodium;icosanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCCC([O-])=O MRQYKJNZWPCFNB-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229940012185 zinc palmitate Drugs 0.000 description 1
- ODNJVAVDJKOYFK-GRVYQHKQSA-L zinc;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Zn+2].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O.CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O ODNJVAVDJKOYFK-GRVYQHKQSA-L 0.000 description 1
- LPEBYPDZMWMCLZ-CVBJKYQLSA-L zinc;(z)-octadec-9-enoate Chemical compound [Zn+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O LPEBYPDZMWMCLZ-CVBJKYQLSA-L 0.000 description 1
- GJAPSKMAVXDBIU-UHFFFAOYSA-L zinc;hexadecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCC([O-])=O GJAPSKMAVXDBIU-UHFFFAOYSA-L 0.000 description 1
- CCTYJGNBCQQCKM-UHFFFAOYSA-L zinc;icosanoate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCCCC([O-])=O CCTYJGNBCQQCKM-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Description
Si含有負極活物質と添加剤を混合し、フローファクター>4を満足する混合粉末とする混合工程、
搬送経路を具備する供給装置を用いて、前記混合粉末を炭素被覆装置に搬送する供給工程、
前記炭素被覆装置を用いて、前記Si含有負極活物質を炭素被覆する炭素被覆工程、を含むことを特徴とする。
Si含有負極活物質と添加剤を混合し、フローファクター>4を満足する混合粉末(以下、本発明の混合粉末ということがある。)とする混合工程、
搬送経路を具備する供給装置を用いて、前記混合粉末を炭素被覆装置に搬送する供給工程、
前記炭素被覆装置を用いて、前記Si含有負極活物質を炭素被覆する炭素被覆工程、を含むことを特徴とする。
3CaSi2+6HCl → Si6H6+3CaCl2
Si6H6 → 6Si+3H2↑
σ1:粉体層の破壊包絡線の終点と接するモールの応力円(Mohr’s stress circle)の最大主応力である。予圧密時の最大主応力とも呼ばれる。
f:原点を通るモールの応力円の最大主応力である。単純崩壊応力とも呼ばれる。
Si含有負極活物質と添加剤を含み、フローファクター>4を満足する混合粉末を、搬送経路を具備する供給装置を用いて搬送する方法。
Si含有負極活物質である100質量部のシリコン材料と、添加剤である0.5質量部のステアリン酸アミドとを、容器回転型混合機に投入して、60rpmで混合し、実施例1の混合粉末とした。なお、シリコン材料の安息角は80°であり、レーザー回折式粒度分布測定装置で測定した粒度分布において、シリコン材料のD50は4.291μm、標準偏差は2.9002、粒度分布の相対標準偏差(%)は67.6%であった。
添加剤としてステアリン酸亜鉛を用いた以外は、実施例1と同様の方法で、実施例2の混合粉末を製造した。
添加剤としてステアリン酸リチウムを用いた以外は、実施例1と同様の方法で、実施例3の混合粉末を製造した。
添加剤としてステアリン酸マグネシウムを用いた以外は、実施例1と同様の方法で、実施例4の混合粉末を製造した。
添加剤としてショ糖脂肪酸エステル(商品名:リョートーシュガーエステル、三菱化学フーズ株式会社)を用いた以外は、実施例1と同様の方法で、実施例5の混合粉末を製造した。
添加剤としてステアリン酸カルシウムを用いた以外は、実施例1と同様の方法で、参考例1の混合粉末を製造した。
添加剤としてフュームドシリカ(商品名:アエロジル、日本アエロジル株式会社)を用いた以外は、実施例1と同様の方法で、参考例2の混合粉末を製造した。
添加剤を添加していないシリコン材料そのものを比較例1の粉末とした。
実施例1〜実施例5の混合粉末、参考例1〜2の混合粉末、比較例1の粉末について、下部セル直動法にて、常温での試験を行い、FF値を算出した。また、実施例1〜実施例3の混合粉末については、下部セル直動法にて150℃での試験を行い、FF値を算出した。結果を表3に示す。表3の「−」は未測定を意味する。
実施例1の混合粉末を用いて、以下のとおり、実施例A−1の炭素被覆Si含有負極活物質を製造した。
スクリュー式回転運動式供給装置を用いて、実施例1の混合粉末を1時間当たり100gの速度で炭素被覆装置に供給した。炭素被覆装置としては、ロータリーキルン型の反応器を用いた。実施例1の混合粉末の供給後、スクリュー式回転運動式供給装置を観察したところ、装置内部への混合粉末の付着がほとんど観察されなかった。また、スクリュー式回転運動式供給装置に供給した混合粉末に対する、炭素被覆装置に供給できた混合粉末の割合を回収率として算出したところ、回収率は96%であった。
炭素被覆工程においては、プロパンを15容量%で含む窒素ガス通気下にて、880℃の条件で、Si含有負極活物質に対して炭素被覆を行い、炭素被覆Si含有負極活物質を製造した。なお、反応器の炉芯管は水平方向に配設されており、炭素被覆工程における炉芯管の回転速度は1rpmとした。炉心管の内周壁には邪魔板が配設されており、反応器は炉芯管の回転に伴って邪魔板上に堆積した内容物が所定の高さで邪魔板から落下するように構成され、その構成によって内容物が撹拌される。
実施例2の混合粉末を用いた以外は、実施例A−1と同様の方法で、実施例A−2の炭素被覆Si含有負極活物質を製造した。実施例2の混合粉末の供給後、スクリュー式回転運動式供給装置を観察したところ、装置内部への混合粉末の付着がほとんど観察されなかった。また、実施例A−2において、供給工程の回収率は97%であった。実施例A−2の炭素被覆Si含有負極活物質における炭素比率は5.6質量%であり、炭素被覆の厚みは15nmであった。また、実施例A−2の炭素被覆Si含有負極活物質の安息角は51°であった。
実施例3の混合粉末を用いた以外は、実施例A−1と同様の方法で、実施例A−3の炭素被覆Si含有負極活物質を製造した。実施例3の混合粉末の供給後、スクリュー式回転運動式供給装置を観察したところ、装置内部への混合粉末の付着がほとんど観察されなかった。また、実施例A−3において、供給工程の回収率は88%であった。炭素被覆工程終了後、炭素被覆装置内のタールの量を秤量したところ、6gであった。実施例A−3の炭素被覆Si含有負極活物質における炭素比率は5.6質量%であり、炭素被覆の厚みは15nmであった。また、実施例A−3の炭素被覆Si含有負極活物質の安息角は33°であった。
比較例1の粉末を用いた以外は、実施例A−1と同様の方法で、比較例A−1の炭素被覆Si含有負極活物質を製造した。比較例1の粉末の供給後、スクリュー式回転運動式供給装置を観察したところ、装置内部への粉末の著しい付着が観察された。また、比較例A−1において、供給工程の回収率は34%であった。炭素被覆工程終了後、炭素被覆装置内のタールの量を秤量したところ、12gであった。比較例A−1の炭素被覆Si含有負極活物質における炭素比率は5.6質量%であり、炭素被覆の厚みは15nmであった。また、比較例A−1の炭素被覆Si含有負極活物質の安息角は56°であった。
実施例A−3の炭素被覆Si含有負極活物質を用いて、以下のとおり、実施例B−3のリチウムイオン二次電池を製造した。
実施例A−3の炭素被覆Si含有負極活物質に代えて、比較例A−1の炭素被覆Si含有負極活物質を用いた以外は、実施例B−3と同様の方法で、比較例B−1のリチウムイオン二次電池を製造した。
実施例B−3及び比較例B−1のリチウムイオン二次電池について、温度25℃の条件下、0.1Cにて評価極の対極に対する電圧が0.05Vになるまで充電を行い、次いで、0.1Cにて評価極の対極に対する電圧が0.7Vになるまで放電を行うとの充放電サイクルを、50サイクル繰り返した。
Claims (2)
- Si含有負極活物質と、ステアリン酸リチウム、ステアリン酸亜鉛、ステアリン酸アミドから選択される少なくとも1種を含む添加剤とを混合し、フローファクター>4を満足する混合粉末とする混合工程、
搬送経路を具備する供給装置を用いて、前記混合粉末を炭素被覆装置に搬送する供給工程、
前記炭素被覆装置にて、有機物として飽和脂肪族炭化水素を用いて、前記Si含有負極活物質を炭素被覆する炭素被覆工程、
を含むことを特徴とする炭素被覆Si含有負極活物質の製造方法。 - 前記Si含有負極活物質が、複数枚の板状シリコン体が厚さ方向に積層されてなる構造を有するものである請求項1に記載の製造方法。
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