KR102668203B1 - 음극 및 이를 포함하는 전기화학장치와 전자장치 - Google Patents
음극 및 이를 포함하는 전기화학장치와 전자장치 Download PDFInfo
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- KR102668203B1 KR102668203B1 KR1020217009536A KR20217009536A KR102668203B1 KR 102668203 B1 KR102668203 B1 KR 102668203B1 KR 1020217009536 A KR1020217009536 A KR 1020217009536A KR 20217009536 A KR20217009536 A KR 20217009536A KR 102668203 B1 KR102668203 B1 KR 102668203B1
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- 230000016507 interphase Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 1
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 1
- IGILRSKEFZLPKG-UHFFFAOYSA-M lithium;difluorophosphinate Chemical compound [Li+].[O-]P(F)(F)=O IGILRSKEFZLPKG-UHFFFAOYSA-M 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002409 silicon-based active material Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- RBYFNZOIUUXJQD-UHFFFAOYSA-J tetralithium oxalate Chemical compound [Li+].[Li+].[Li+].[Li+].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O RBYFNZOIUUXJQD-UHFFFAOYSA-J 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 1
- NDZWKTKXYOWZML-UHFFFAOYSA-N trilithium;difluoro oxalate;borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-].FOC(=O)C(=O)OF NDZWKTKXYOWZML-UHFFFAOYSA-N 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
Description
도1A는 실시예1중 규소산화물SiOx의 스캔식전자현미경(SEM) 사진을 나타내고, 도1B는 실시예1중 흑연입자의 SEM사진을 나타내며, 도1C와 도1D는 각각 실시예1중 음극의 일부 단면의 SEM사진을 나타낸다.
도2A는 실시예1중 규소산화물SiOx의 입경분포곡선을 나타내고, 도2B는 실시예1중 흑연의 입경분포곡선을 나타낸다.
도3A는 실시예1과 비교예1중 리튬이온전지의 사이클감쇠 곡선이고, 도3B는 실시예1과 비교예1의 전지변형 곡선이고, 도3C는 실시예10중 음극활성재료의 X선회절(XRD)도이며, 도3D는 비교예4중 음극활성재료의 X선회절도이다.
도4는 본 출원의 하나의 실시예의 음극활성재료의 구조설명도를 나타낸다.
도5는 본 출원의 다른 하나의 실시예의 음극활성재료의 구조설명도를 나타낸다.
Claims (52)
- 규소기입자와 흑연입자를 포함하고,
상기 규소기입자의 가장자리와의 수직거리가 0-6μm인 범위내에 존재하는 흑연입자수가 N이며,
상기 규소기입자의 총수량을 기준으로, 50%보다 큰 규소기입자는 6≤N≤17을 만족하며,
상기 규소기입자의 가장자리와의 수직거리가 0-6μm인 범위내에 존재하는 흑연입자수 N의 측정방법은,
Ar입자를 채용하여 음극단면을 연마하고, 이후 SEM을 채용하여 가장자리가 집전체 및 음극표면와의 최소거리가 6μm보다 작지 않은 규소기입자 중에서 적어도 30개 규소기입자를 한번에 촬영하고, 상기 적어도 30개 규소기입자 가장자리와의 수직거리가 0-6μm인 범위내에 존재하는 흑연입자수 N을 기록하는 것으로 수행되고, 여기서 흑연입자수는 단일 흑연입자의 개수이고, 즉 일차흑연입자의 개수를 가리키며, 상기 N개 흑연입자 중의 각 흑연입자는 전부가 상기 적어도 30개 규소기입자 가장자리와의 수직거리가 0-6μm인 범위내에 있을 수 있고, 또한 일부 중의 각 흑연입자는 전부 상기 범위내에 있고 다른 일부 중의 각 흑연입자는 일부만 상기 범위내에 있을 수 있으며,
상기 규소기입자는 규소복합물 기질과 산화물MeOy층을 포함하고, 상기 산화물MeOy층은 상기 규소복합물 기질의 적어도 일부을 코팅하고 있으며, 여기서, Me는 Al, Si, Mn, V, Cr, 또는 Co 중의 적어도 일종을 포함하고, y는 0.5-3이며, 상기 산화물MeOy층은 탄소재료를 포함하는 것을 특징으로 하는 음극. - 제1항에 있어서,
상기 규소기입자는 X선회절도에서 2θ가 28.0°-29.0°인 범위내에서의 최고강도수치는 I2이고, 20.5°-21.5°인 범위내에서의 최고강도수치는 I1이며,
여기서, 0<I2/I1≤1인 것을 특징으로 하는 음극. - 제1항에 있어서,
상기 규소기입자의 입경분포가 0.3≤Dn10/Dv50≤0.6을 만족하는 것을 특징으로 하는 음극. - 제1항에 있어서,
Me는 Ti 또는 Zr중의 적어도 일종을 더 포함하는 것을 특징으로 하는 음극. - 삭제
- 제4항에 있어서,
상기 규소기입자는 폴리머층을 더 포함하고,
상기 폴리머층은 상기 산화물MeOy층의 적어도 일부을 코팅하고 있으며,
상기 폴리머층은 탄소재료를 포함하는 것을 특징으로 하는 음극. - 제1항에 있어서,
상기 흑연입자의 평균구형도는 A이고,
상기 규소기입자의 평균구형도는 B이며,
A와 B는 0<B-A≤0.3을 만족하는 것을 특징으로 하는 음극. - 제4항 또는 제6항에 있어서,
상기 규소복합물 기질은 SiOx을 포함하고,
0.6≤x≤1.5인 것을 특징으로 하는 음극. - 제4항 또는 제6항에 있어서,
상기 규소복합물 기질은 나노Si결정립, SiO, SiO2 또는 그 임의의 조합을 포함하는 것을 특징으로 하는 음극. - 제9항에 있어서,
상기 나노Si결정립의 사이즈는 100nm보다 크지 않은 것을 특징으로 하는 음극. - 제4항 또는 제6항에 있어서,
상기 산화물MeOy층의 두께는 0.5nm-1000nm인 것을 특징으로 하는 음극. - 제4항 또는 제6항에 있어서,
상기 규소기입자의 총중량을 기준으로, Me원소의 중량백분율이 0.005wt%-1wt%인 것을 특징으로 하는 음극. - 제6항에 있어서,
상기 폴리머층은 폴리불화비닐리덴 및 그 유도체, 카르복시메틸셀룰로오스 및 그 유도체, 나트륨카르복시메틸셀룰로오스 및 그 유도체, 폴리비닐피롤리돈 및 그 유도체, 폴리아크릴산 및 그 유도체, 폴리스티렌부타디엔 고무, 폴리아크릴아미드, 폴리이미드, 폴리아미드이미드 또는 그 임의의 조합을 포함하는 것을 특징으로 하는 음극. - 제6항에 있어서,
상기 규소기입자의 총중량을 기준으로, 상기 폴리머층의 중량백분율이 0.05-5wt%인 것을 특징으로 하는 음극. - 제6항에 있어서,
상기 폴리머층의 두께는 1nm-100nm인 것을 특징으로 하는 음극. - 제4항 또는 제6항에 있어서,
상기 탄소재료는 탄소나노튜브, 탄소나노입자, 탄소섬유, 그래핀 또는 그 임의의 조합을 포함하는 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
상기 규소기입자의 입경Dv50이 2.5-10μm인 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
상기 규소기입자의 비표면적이 1-50m2/g인 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
상기 규소기입자의 평균구형도가 0.8-1.0인 것을 특징으로 하는 음극. - 제19항에 있어서,
구형도가 0.8보다 낮은 규소기입자수가 규소기입자 총수량중에서 차지하는 백분율이 10%보다 크지 않은 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
상기 흑연입자의 평균구형도가 0.5-0.8인 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
구형도가 0.5-0.8인 흑연입자수가 흑연입자 총수량중에서 차지하는 백분율이 95%보다 작지 않은 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
라만 스펙트럼 분석중에서, 상기 흑연입자는 1330cm-1에서 회절피크I1330을 가지고, 1580cm-1에서 회절피크I1580을 가지며,
I1330/I1580의 비는 0.7<I1330/I1580<2.0을 만족하는 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
상기 흑연입자의 입경Dv50이 0.01-80μm인 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
상기 흑연입자의 비표면적이 30m2/g보다 크지 않은 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 있어서,
상기 흑연입자의 OI값이 1-30인 것을 특징으로 하는 음극. - 제1항 내지 제4항, 제6항, 및 제7항 중 어느 한 항에 따른 음극을 포함하는 것을 특징으로 하는 전기화학장치.
- 제27항에 있어서,
리튬이온전지인 것을 특징으로 하는 전기화학장치. - 제28항에 따른 전기화학장치를 포함하는 것을 특징으로 하는 전자장치.
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