CN102405543A - 金属表面的化学保护 - Google Patents
金属表面的化学保护 Download PDFInfo
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- CN102405543A CN102405543A CN2010800161268A CN201080016126A CN102405543A CN 102405543 A CN102405543 A CN 102405543A CN 2010800161268 A CN2010800161268 A CN 2010800161268A CN 201080016126 A CN201080016126 A CN 201080016126A CN 102405543 A CN102405543 A CN 102405543A
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- carbon
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- 229910052751 metal Inorganic materials 0.000 title description 10
- 239000002184 metal Substances 0.000 title description 10
- 239000000126 substance Substances 0.000 title description 7
- 239000002243 precursor Substances 0.000 claims abstract description 40
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 27
- 239000001301 oxygen Substances 0.000 claims abstract description 27
- 239000007769 metal material Substances 0.000 claims abstract description 23
- 239000010410 layer Substances 0.000 claims abstract description 21
- 239000011241 protective layer Substances 0.000 claims abstract description 20
- 239000003792 electrolyte Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 108
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 77
- 229910052736 halogen Inorganic materials 0.000 claims description 66
- 150000002367 halogens Chemical group 0.000 claims description 66
- 125000003118 aryl group Chemical group 0.000 claims description 44
- 125000003545 alkoxy group Chemical group 0.000 claims description 41
- -1 n-pro-pyl Chemical group 0.000 claims description 41
- 150000001875 compounds Chemical class 0.000 claims description 32
- 125000000217 alkyl group Chemical group 0.000 claims description 25
- 229910052744 lithium Inorganic materials 0.000 claims description 22
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052698 phosphorus Inorganic materials 0.000 claims description 10
- 239000011574 phosphorus Substances 0.000 claims description 10
- 125000002347 octyl 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])[H] 0.000 claims description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 6
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052794 bromium Inorganic materials 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 4
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 4
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 4
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 4
- 125000002704 decyl group Chemical group [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])* 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 239000011630 iodine Substances 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 125000001400 nonyl 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])[H] 0.000 claims description 4
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 4
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 4
- 125000002948 undecyl 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])[H] 0.000 claims description 4
- 150000001491 aromatic compounds Chemical class 0.000 claims description 3
- 150000002902 organometallic compounds Chemical class 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 210000004027 cell Anatomy 0.000 description 12
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- HMIVSEUZMDMVFB-UHFFFAOYSA-N C(C)(C)PC(C)C.[Cl] Chemical compound C(C)(C)PC(C)C.[Cl] HMIVSEUZMDMVFB-UHFFFAOYSA-N 0.000 description 3
- USNQINRPCUUARI-UHFFFAOYSA-N C(C)PCC.[Cl] Chemical compound C(C)PCC.[Cl] USNQINRPCUUARI-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
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- 229910052782 aluminium Inorganic materials 0.000 description 3
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- 125000001424 substituent group Chemical group 0.000 description 2
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- HWPLJWHPJDICQU-UHFFFAOYSA-N BrC(BC)Br Chemical compound BrC(BC)Br HWPLJWHPJDICQU-UHFFFAOYSA-N 0.000 description 1
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- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- OHBTULDTCSOWOY-UHFFFAOYSA-N [C].C=C Chemical compound [C].C=C OHBTULDTCSOWOY-UHFFFAOYSA-N 0.000 description 1
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- 238000000354 decomposition reaction Methods 0.000 description 1
- WDIIYWASEVHBBT-UHFFFAOYSA-N di(propan-2-yl)phosphane Chemical compound CC(C)PC(C)C WDIIYWASEVHBBT-UHFFFAOYSA-N 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 150000003462 sulfoxides Chemical class 0.000 description 1
- 230000008961 swelling Effects 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
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
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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
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
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- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
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Abstract
一种电化学单元包含有具有含氧层的金属材料的阳极。该电化学单元还包含阴极和电解质。该阳极包含通过使D或P区前体与含氧层反应而形成的保护层。
Description
相关申请
本申请要求2009年3月2号提交的美国专利申请12/396,223的优先权，通过引用将其并入本文。
技术领域
本发明涉及金属表面的化学保护。
背景技术
现有技术已知包含金属阳极、阴极和固体或包含溶剂的电解质的电化学单元(cell)。这样的蓄电池在重复充电/放电循环中具有限制，并且当与它们的初始充电和放电容量相比时，在它们的充电和放电容量方面可有所降低。此外，固体蓄电池的初始容量经常低于所需要的。因此，现有技术中存在对具有高初始容量并在重复的充电和放电循环中维持这样的容量的改良蓄电池的需求。
与电化学单元相关的另一个问题是在重复充电和放电循环中枝晶的产生。当电化学单元充电时，枝晶可在阳极上形成。枝晶可在重复的循环中生长并且导致蓄电池下降的性能或不允许蓄电池充电和放电的短路。因此，现有技术中存在对具有改善的循环寿命并限制枝晶形成的蓄电池和电极的需求。
发明内容
电化学单元包含具有金属材料的阳极，该金属材料具有含氧层。该电化学单元还包含阴极和电解质。该阳极包含通过使D或P区前体与含氧层反应而形成在金属材料上的保护层。
附图说明
图1是在施加保护层之前和之后锂金属的波长与强度的IR光谱曲线；
图2是具有保护层的锂金属的差示扫描量热曲线；
图3用于阻抗测试的实验装置的图表；
图4形成保护层的三甲基氯硅烷前体和参照材料的阻抗曲线；
图5形成保护层的氯二异丙基膦前体和参照材料的阻抗曲线；
图6形成保护层的氯二乙基膦前体和参照材料的阻抗曲线；
图7形成保护层的溴二甲基硼烷(dromodimethylborane)前体和参照材料的阻抗曲线；
图8是形成保护层的三甲基氯硅烷、氯二异丙基膦、氯二乙基膦和溴二甲基硼烷和参照材料的阻抗曲线；
图9是形成保护层的四乙基原硅酸酯前体和参照材料的阻抗曲线；
图10是显示在金属表面上沉积的厚层的横截面SEM数据；
图11用于实施例4的实验装置的描述。
具体实施方式
在本文中使用的术语电化学单元意指具有阳极、阴极和插入两者之间的离子导电电解质的装置。该电化学单元可为蓄电池、电容器或其它这样的装置。蓄电池可具有一次或二次化学性质。蓄电池可具有固体电解质或液体电解质。在本文中使用的术语阳极意指在放电循环期间氧化的电极。
公开了具有包含金属材料的阳极的电化学单元，该金属材料具有含氧层。阳极材料可为如元素周期表所指出的碱金属或碱土金属。金属材料的非限制性例子包括：锂、铝、钠和镁。在本发明的一个优选方面，金属材料为锂。
含氧层可通过将金属材料暴露于气氛中形成或可以以其它方式形成于金属材料上。电化学单元还包含阴极，其可由任何合适的材料形成。电解质置入在阳极和阴极之间，并且其可为任何合适的形式，包括固体电解质液体电解质和凝胶聚合物电解质，该凝胶聚合物电解质是用溶剂和盐溶胀的聚合物基体。固体电解质可为聚合物类型、无机层或这两者的混合物。聚合物电解质的例子包括PEO基和PEG基的聚合物。无机电解质可由硫化物玻璃、磷化物玻璃、氧化物玻璃及其混合物组成。液体电解质的例子包括具有溶解的金属离子盐的碳酸酯溶剂，例如在乙烯碳/碳酸乙酯(EC/DEC)中的1M LiPF6。
电化学单元的阳极包括通过使D或P区前体与含氧层反应而形成于其上的化学键合的保护层。术语D或P区前体包括具有在元素周期表的D或P区中的元素的化合物。D或P区元素的例子包括磷、硼、硅、钛、钼、钽、钒等。D或P区前体可为有机金属化合物。有机金属化合物的例子包括：金属间化合物、具有键合于其上的有机取代基的合金和金属。在本发明的一个优选方面，D或P区前体可包括硅、硼或磷。D或P区前体与金属材料的含氧层反应以形成保护层。
在一个实施方案中，D或P区前体可以是具有以下式的化学化合物：AR1R2X，其中A选自磷或硼，X是卤素或包含卤素的化合物，并且R1选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基。R2选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基。
卤素可包括氯、溴、氟和碘。烷基、烷氧基和芳基可为氟化或部分氟化的。
烷基可为甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、叔戊基、异辛基、叔辛基、2-乙基己基、壬基、癸基、十一烷基、环戊基、环己基、环庚基、环辛基、1-甲基环戊基、1-甲基环己基、1-甲基环己基和1-甲基-4-异丙基环己基，尽管本发明也可使用没有列出的其它烷基。还可使烷基官能化。合适的官能团包括：醚、硫醚、亚砜等。
芳基可为苯基，在对、间或邻位上具有烷基取代基的苯基和多环芳族化合物(polyaromatic compound)。合适的多环芳族化合物的例子包括萘的衍生物。
在本发明的另一个实施方案中，D或P区前体可以是具有以下式的化学化合物：AR1R2R3R4X，其中A为磷，X为卤素或包含卤素的化合物，并且R1选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基、或氧，R2选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基、或氧，R3选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳原子的芳基、或氧，R4选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳原子的芳基、或氧。
在化合物包含双键氧或其它双键取代基的情况下，R基的数目总数可少于4。
如同前面描述的实施方案，卤素、烷基、烷氧基和芳基相同并且不再重复。
在本发明的另一个实施方案中，D或P区前体可以是具有以下式的化学化合物：SiR1R2R3X，其中X为卤素或包含卤素的化合物，并且R1选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R2选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基、R3选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳原子的芳基。
如同前面描述的实施方案，卤素、烷基、烷氧基和芳基相同并且不再重复。
在另一个方面，化学保护层可不键合于如上所述的金属材料。在该申请中，电化学单元的阳极还由通过使D或P区前体与含氧层反应而在其上形成保护层所覆盖。D或P区前体可包括如上所述的相同类型的材料，包括：具有以下式的化合物：AR1R2X，其中A选自磷或硼，X是卤素或包含卤素的化合物，并且R1选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R2选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基；具有以下式的化合物：AR1R2R3R4X，其中A为磷，X为卤素或包含卤素的化合物，并且R1选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基、或氧，R2选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基、或氧，R3选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基、或氧，R4选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基、或氧；以及具有以下式的化学化合物：SiR1R2R3X，其中X为卤素或包含卤素的化合物，并且R1选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R2选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R3选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳原子的芳基。
除了上述确定的化合物之外，另外的含氧物质还可包含于D或P区前体，并且反应形成化学保护层。合适的含氧物质可包括：氧、水蒸汽和其它含氧的化合物。
在化学保护层不键合于金属材料的表面的实施方案中，D或P区前体与金属材料的含氧层和/或与任何另外的含氧物质反应以引发D或P区前体的分解、水解、聚合或其它反应，从而形成不键合于金属材料表面的层。
实施例
在实施例部分详细描述的实验中，将锂金属条带暴露于各种前体化合物。在室温下于包含前体化合物的惰性气氛中，将锂条带放置在密封烧瓶中。使条带暴露于前体合适周期的时间，用于前体与在锂上的金属含氧层反应以形成保护层。对各种样品进行各种分析程序：阻抗测试、IR光谱测试和差示扫描量热测试。
实施例1
如图1所示，采用IR光谱分析锂金属的未处理样品和根据上述的步骤用三甲基氯硅烷处理240秒的样品。对于未处理样品，对应氢氧化锂键的峰显示于3600cm-1范围内。对于处理过的样品没有显示该峰，该样品包括对应硅氧键在1100cm-1范围内的峰。该关系说明前体化合物已经与含氧金属反应以形成硅氧键。
实施例2
如图2所示，采用差示扫描量热分析锂金属的未处理样品和根据上述的步骤用三甲基氯硅烷处理的样品。将样品放置在铝盘中，使氮气围绕样品流动。将样品重复地加热到高于熔点并且冷却到低于熔点，以确定锂是否受到保护免于环境影响。未处理的锂样品与铝盘反应并且没有显示代表纯锂金属的熔化和凝固。未处理的样品，如图2所示，在锂的熔点或非常接近锂的熔点处展现了非常清晰的熔化和凝固(在熔点处微量的过热或过冷取决于加热速率)。窄峰说明锂金属得到保护并且与未保护的样品相比没有与环境反应。
实施例3
对各种处理过的锂样品和作为参照的未处理的锂进行阻抗测试。使用的实验装置显示于图3中。使用如上所述的步骤形成各种样品。在正电极位置放置有样品的实验装置中测试锂样品。不同样品的阻抗曲线显示于图4-7中。图4显示了用三甲基氯硅烷前体处理形成保护层的样品的阻抗曲线。图5显示了对于形成保护层的氯二异丙基膦前体的阻抗曲线。图6显示了对于形成保护层的氯二乙基膦前体的阻抗曲线。图7显示了对于形成保护层的二溴二甲基硼烷(dibromodimethylborane)前体的阻抗曲线。如从附图中可看出，处理过的样品均具有斜率小于参照样品的阻抗曲线。该行为显示了相对于未处理样品的改善的性能。使用阻抗值来计算各种样品的阻抗，对于各种样品的阻抗显示于图8中。如从附图中可看出，所有处理过的样品的阻抗小于未处理的参照物。前体材料的各种元素和R基对样品的阻抗具有影响。氯二异丙基膦样品显示了处理的样品的最低阻抗。对于用作电化学单元中的阳极，需要较低阻抗的金属材料。
实施例4
分析了锂金属的未处理样品和根据上述的步骤用四乙基原硅酸酯处理的样品。对锂的处理过和作为参照的未处理的锂进行阻抗测试。使用的实验装置显示于图11中。使用阻抗曲线来计算样品的阻抗，其显示于图9中。如从附图中可看出，所有处理过的样品的阻抗小于未处理的参照物。对于用作电化学单元中的阳极，需要较低阻抗的金属材料。
参考图10，显示了处理过的样品的横截面的SEM显微照片。如从显微照片中可看出，化学保护层为厚层，如层的厚度所证明的那样，该厚层没有化学键合于金属表面。
已经以说明性方式描述了本发明。将理解所使用的术语意欲为描述词语的本义而不是限制。在考虑到以上的教导下本发明的许多修改或改变是可能的。因此，在所附的权利要求的范围内，可在如特别描述之外实践本发明。
Claims (25)
1.用于电化学单元的阳极，包含：
具有含氧层的金属材料；
通过使D或P区前体与含氧层反应而在金属材料上形成的保护层。
2.权利要求1的阳极，包括将含氧物质添加到D或P区前体。
3.权利要求1的阳极，其中D或P区前体为有机金属化合物。
4.权利要求1的阳极，其中金属材料选自碱金属和碱土金属。
5.权利要求1的阳极，其中金属材料包含锂。
6.权利要求1的阳极，其中D或P区前体包含具有以下式的化学化合物：AR1R2X，其中A选自磷或硼，X是卤素或包含卤素的化合物，并且R1选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R2选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基。
7.权利要求6的阳极，其中卤素选自氯、溴、氟和碘。
8.权利要求6的阳极，其中烷基、烷氧基和芳基可为氟化或部分氟化的。
9.权利要求6的阳极，其中烷基是官能化的。
10.权利要求6的阳极，其中烷基选自甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、叔戊基、异辛基、叔辛基、2-乙基己基、壬基、癸基、十一烷基、环戊基、环己基、环庚基、环辛基、1-甲基环戊基、1-甲基环己基、1-甲基环己基和1-甲基-4-异丙基环己基。
11.权利要求6的阳极，其中芳基选自苯基，在对、间或邻位上具有烷基取代基的苯基和多环芳族化合物。
12.权利要求1的阳极，其中D或P区前体包含具有以下式的化学化合物：AR1R2R3R4X，其中A为磷，X为卤素或包含卤素的化合物，并且R1选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基，具有1-20个碳的芳基、或氧，R2选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基，具有1-20个碳的芳基、或氧，R3选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基、或氧，R4选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基，或氧。
13.权利要求12的阳极，其中卤素选自氯、溴、氟和碘。
14.权利要求12的阳极，其中烷基、烷氧基和芳基可为氟化或部分氟化的。
15.权利要求12的阳极，其中烷基是官能化的。
16.权利要求12的阳极，其中烷基选自甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、叔戊基、异辛基、叔辛基、2-乙基己基、壬基、癸基、十一烷基、环戊基、环己基、环庚基、环辛基、1-甲基环戊基、1-甲基环己基、1-甲基环己基和1-甲基-4-异丙基环己基。
17.权利要求1的阳极，其中D或P区前体包含具有以下式的化学化合物：SiR1R2R3X，其中X为卤素或包含卤素的化合物，并且R1选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R2选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R3选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基。
18.权利要求17的阳极，其中卤素选自氯、溴、氟和碘。
19.权利要求17的阳极，其中烷基、烷氧基和芳基可为氟化或部分氟化的。
20.权利要求17的阳极，其中烷基是官能化的。
21.权利要求17的阳极，其中烷基选自甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、叔戊基、异辛基、叔辛基、2-乙基己基、壬基、癸基、十一烷基、环戊基、环己基、环庚基、环辛基、1-甲基环戊基、1-甲基环己基、1-甲基环己基和1-甲基-4-异丙基环己基。
22.一种电化学单元，包含：
包括具有含氧层的金属材料的阳极；
阴极；
电解质；
阳极包括通过使D或P区前体与含氧层反应而在金属材料上形成的保护层。
23.权利要求22的电化学单元，其中D或P区前体包含具有以下式的化学化合物：AR1R2X，其中A选自磷或硼，X是卤素或包含卤素的化合物，并且R1选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R2选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基。
24.权利要求22的电化学单元，其中D或P区前体包含具有以下式的化学化合物：AR1R2R3R4X，其中A为磷，X为卤素或包含卤素的化合物，并且R1选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基、或氧，R2选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基，具有1-20个碳的芳基、或氧，R3选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基、或氧，R4选自卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基、具有1-20个碳的芳基、或氧。
25.权利要求22的电化学单元，其中D或P区前体包含以下式的化学化合物：SiR1R2R3X，其中X为卤素或包含卤素的化合物，并且R1选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R2选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基，R3选自氢、卤素、具有1-20个碳的烷基、包含1-20个碳的烷氧基或具有1-20个碳的芳基。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US12/396,223 | 2009-03-02 | ||
| US12/396,223 US20090220857A1 (en) | 2005-09-02 | 2009-03-02 | Chemical protection of metal surface |
| PCT/US2010/025828 WO2010101856A1 (en) | 2009-03-02 | 2010-03-02 | Chemical protection of metal surface |
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| CN102405543B CN102405543B (zh) | 2015-07-22 |
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| US (3) | US20090220857A1 (zh) |
| JP (1) | JP2012519368A (zh) |
| KR (1) | KR101720660B1 (zh) |
| CN (1) | CN102405543B (zh) |
| WO (1) | WO2010101856A1 (zh) |
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| DE102013200414A1 (de) | 2012-01-13 | 2014-01-09 | Chemetall Gmbh | Phosphorbeschichtete Lithiummetallprodukte, Verfahren zu deren Herstellung und Verwendung |
| WO2013104787A1 (de) | 2012-01-13 | 2013-07-18 | Chemetall Gmbh | Stabilisierte mit legierungsbildenden elementen beschichtete lithiummetallabformungen und verfahren zu deren herstellung |
| CN105392737B (zh) | 2013-04-19 | 2018-05-18 | 罗克伍德锂有限责任公司 | 用含氮壳涂敷的稳定化的锂金属结构及其制造方法 |
| CN104152326B (zh) * | 2014-08-30 | 2017-08-25 | 枣庄新华酒业有限公司 | 一种浓香型大曲酒生产工艺 |
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| JP4501344B2 (ja) * | 2003-01-23 | 2010-07-14 | ソニー株式会社 | 二次電池 |
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- 2010-03-02 JP JP2011553014A patent/JP2012519368A/ja active Pending
- 2010-03-02 CN CN201080016126.8A patent/CN102405543B/zh not_active Expired - Fee Related
- 2010-03-02 KR KR1020117023068A patent/KR101720660B1/ko active IP Right Grant
-
2014
- 2014-01-15 US US14/156,241 patent/US20140134488A1/en not_active Abandoned
- 2014-10-14 US US14/513,507 patent/US20150026967A1/en not_active Abandoned
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| US5314765A (en) * | 1993-10-14 | 1994-05-24 | Martin Marietta Energy Systems, Inc. | Protective lithium ion conducting ceramic coating for lithium metal anodes and associate method |
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| US20080069944A1 (en) * | 2006-09-19 | 2008-03-20 | Toyota Engineering & Manufacturing North America, Inc. | Method of chemical protection of metal surface |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2012519368A (ja) | 2012-08-23 |
| US20090220857A1 (en) | 2009-09-03 |
| KR101720660B1 (ko) | 2017-03-28 |
| US20140134488A1 (en) | 2014-05-15 |
| CN102405543B (zh) | 2015-07-22 |
| WO2010101856A1 (en) | 2010-09-10 |
| US20150026967A1 (en) | 2015-01-29 |
| KR20120028297A (ko) | 2012-03-22 |
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