CN1302568C - 生产用作可再充电的锂电池的正电极的电极材料的方法 - Google Patents
生产用作可再充电的锂电池的正电极的电极材料的方法 Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 26
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011572 manganese Substances 0.000 claims abstract description 10
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims abstract description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 5
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 4
- PPTSBERGOGHCHC-UHFFFAOYSA-N boron lithium Chemical compound [Li].[B] PPTSBERGOGHCHC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 229910052810 boron oxide Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- -1 boron oxide compound Chemical class 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 7
- 229910052796 boron Inorganic materials 0.000 abstract description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 6
- 239000004411 aluminium Substances 0.000 abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052723 transition metal Inorganic materials 0.000 abstract description 4
- 150000003624 transition metals Chemical class 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 230000007613 environmental effect Effects 0.000 description 6
- 229910000314 transition metal oxide Inorganic materials 0.000 description 4
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 3
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical class [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910013292 LiNiO Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- STUKNTHDFYCZOR-UHFFFAOYSA-N [Ba+2].[O-2].[Li+] Chemical compound [Ba+2].[O-2].[Li+] STUKNTHDFYCZOR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910000103 lithium hydride Inorganic materials 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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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- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
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- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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Abstract
本发明涉及基于锂-过渡金属氧化物，用作可重复充电的锂-电池的正电极的电极材料，锂-过渡金属氧化物是一种具有至少两种过渡金属(例如镍和/或锰)的锂-过渡金属氧化物，并且具有层结构和被掺杂(例如用铝和/或硼)。此电极材料呈现高的重复使用稳定性，并且可廉价地生产。
Description
技术领域
本发明涉及一种生产用作可重复充电的锂电池的正电极的电极材料的方法。
背景技术
EP 0918041公开了一种具有层结构的电极材料，它含有过渡金属Ni和Co作为主要成份，并且通过掺杂Al，Fe，Mn和B而被稳定。EP 0696075公开了用钴作为主要成份的电极材料。
可充电的锂电池主要应用于便携式电子设备中，如电信终端，计算机和放像装置中。这些应用对电池有高的要求。主要是单位体积和/或重量应存贮尽可能多的能量。此外它还应具有安全性和环境相容性。因而高能量密度和高的额定能量是对这种电池的电极材料提出的两个基本要求。
对这种电极材料的另一个主要要求是重复使用的稳定性，其中一次重复使用包含一次充电和一次放电过程。重复使用的稳定性主要决定于在多次重复使用之后可提供使用的额定充电。在假设每次重复使用时重复使用的稳定性为99％时可能在重复使用100次后可提供使用的额定充电仅为开始时的数值的37％。因此如此相对高的99％的数值仍是不够的。上述方式的一个可重复充电的合适的高效率电池不仅应能在尽可能小的重量和体积下存贮规定的能量，而且也应可以数百次地放电和再充电。这里起决定性作用的是电极材料。
基于这种电池的重大的经济意义，已经做了许多努力来寻找用于电极的材料，它保证尽可能地满足上述要求。
至今用作可重复充电的锂电池的正电极的材料的主要是应用过渡金属氧化物或-硫化物，有机分子和聚合物。实际中证实过渡金属氧化物和硫化物是特别适合的。这些材料被称为存入-或插入-电极材料，并且存在于许多空间温度的可重复充电的电池。进一步推广这种材料的理由在于电化存贮反应是简单而且可逆的。
基于锂-存贮反应的可重复充电电池的方案在1970年已经形成了，并且在其间的时间内建议了大量采用此原理的电极，锂-电池的可重复充电性主要依据在存入-和放出Li+时气体材料的尺寸稳定性。
作为用于正电极的可逆材料，如上所述的过渡金属氧化物已公开。它主要是锂钴氧化物，锂镍氧化物，锂锰氧化物和锂钒氧化物。但是这些材料部分是不合适的。锂钴氧化物相对较贵，且不是特别环境相容的。锂锰氧化物可能由于环境相容性而特别适用。然而业已表明，这些氧化物通常具有尖晶石结构，因而有低的充电性能或在远离锂的地方不稳定。研究表明，正交晶的锂锰氧化物在锂的伸展区过渡到一个尖晶石结构。这里现有技术的相关出版物有：Martin Winter，Jürgen O.Besenhard，Michael E.Spahr和Petr Novak的文章“用于可重复充电的锂电池的插入电极材料”，ADVANCED MATERIALS，1998年11月10日第10期，第725至763页，以及M.E.Spahr的文章“新型氧化物，碳化合物，硅化物及毫微米结构材料的合成和特性化以及它们的电化和磁化研究”，ETH论文，12281号。
发明内容
本发明的目的在于提供上述类型的电极材料，其特征在于高的重复稳定性，它不仅能廉价生产，而且适用于生产可重复使用的高效电池。而且此电极材料有相对较好的环境相容性。
本发明的任务这样来完成：生产用作具有层结构的可重复充电的锂电池的正电极的电极材料的方法，所述电极材料基于锂过渡金属氧化物，所述方法包括：-使锰和/或镍的乙酸盐、硝酸盐或氢氧化物与LiOBr进行反应，以形成沉淀，其中[摩尔Li∶(摩尔Mn+摩尔Ni)]的比率为1∶1，-将所述沉淀洗涤并干燥至少一次，-向所述沉淀加入LiOH，-在低于900℃的温度下，在氧化环境中将所述沉淀加热4至48小时。研究表明，采用本发明的电极材料可生产正电极，它们经过数百次重复使用还是稳定的，或者优化了充电性能。这个高的重复使用稳定性是突出的，它结束了多年来持续的为改善锂-电池材料所做的努力。更高的重复使用稳定性可延长电池的寿命。
利用锰对于环境相容性是特别有好处的。锰比钴有明显好的环境相容性，并且也是廉价的。在相对高的锰成份时电极材料也是稳定的。
按照本发明的另一设计，锂过渡金属氧化物具有掺杂的铝和/或硼。掺杂了铝和/或硼的过渡金属氧化物形成了特别好的重复使用稳定性。此掺杂可用现有方法通过用盐沉淀实现。特别有优点的是掺杂硼氧化物，硼酸或锂硼氢化物。锂硼氢化物干燥地加入，并且在掺杂硼时加入的质子可能远离。用铝和硼混合掺杂也是合适的。
最好锂过渡金属氧化物用5-15Mol％掺杂。
本发明其它有优点的特征由相关权利要求给出并在下面被说明。
合适的电极材料具有类似于LiNiO2的二维层结构，并且具有公共的化学式Li(MI)(MII)O2，其中M是一个过渡金属。它最好是金属锰和另一种金属镍。在化学式Li(MnxNi1-x)O2中x在0.05至0.5的范围内。这样本发明电极材料具有一个层结构。尖晶石结构被消除了。少量(＜0.05)的另一种过渡金属可以产生有利的影响。
掺杂以现有的方法通过沉淀实现。特别适用的是硼氧化物，硼酸或锂硼氢化物。同样用铝的掺杂是有优点的。铝和硼可以单独地或以不同比例被掺杂。
具有化合物LiMn0.5Ni0.4Al0.1O2的电极材料已被生产和试验。该电极材料作为正电极相对于规定的充电(安培小时/公斤)具有超过200次重复使用的稳定性。规定充电为约140安培小时/公斤的常数。
附图说明
图2示出一个典型的铝-掺杂标本的电化重复使用性能。充电范围平均在3.9和4伏间。图1示出相应的静电流放电曲线。
具体实施方式
因而本发明建议了一种电极材料，它不仅稳定，而且也可廉价地生产和进一步有利于环保。
在典型的合成中，溶于水的金属盐(例如硝酸盐、乙酸盐或氢氧化物)与等摩尔量的LiOBr溶液进行反应。形成的沉淀被多次洗涤、干燥并掺入氢化锂。少量过剩的锂，例如相对于金属成份1.2倍的锂是有利的。固态的样本在氧化环境中、最好是在氧气中加热4小时至2天。固态样本加热的温度最好低于900℃，最好约为800℃。已经表明，大大高于900℃的温度会损伤其应用性能。
Claims (3)
1.生产用作具有层结构的可重复充电的锂电池的正电极的电极材料的方法，所述电极材料基于锂过渡金属氧化物，所述方法包括：
-使锰和/或镍的乙酸盐、硝酸盐或氢氧化物与LiOBr进行反应，以形成沉淀，其中
[摩尔Li∶(摩尔Mn+摩尔Ni)]的比率为1∶1，
-将所述沉淀洗涤并干燥至少一次，
-向所述沉淀加入LiOH，
-在低于900℃的温度下，在氧化环境中将所述沉淀加热4至48小时。
2.如权利要求1所述的生产电极材料的方法，其特征在于，锂过渡金属氧化物借助于锂硼氢化物，硼酸和/或硼氧化物被掺杂。
3.如权利要求1所述的方法，其特征在于，锂过渡金属氧化物至少部分掺杂铝。
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| JP (1) | JP2003515911A (zh) |
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| CN (1) | CN1302568C (zh) |
| AT (1) | ATE306122T1 (zh) |
| AU (1) | AU1506901A (zh) |
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| GB0117235D0 (en) * | 2001-07-14 | 2001-09-05 | Univ St Andrews | Improvements in or relating to electrochemical cells |
| AU2008203082B2 (en) * | 2001-07-14 | 2011-01-06 | The University Court Of The University Of St Andrews | Improvements in or relating to electrochemical cells |
| JP3873717B2 (ja) * | 2001-11-09 | 2007-01-24 | ソニー株式会社 | 正極材料およびそれを用いた電池 |
| US7217406B2 (en) * | 2002-02-21 | 2007-05-15 | Tosoh Corporation | Lithium-manganese composite oxide granular secondary particle, method for production thereof and use thereof |
| NZ520452A (en) | 2002-10-31 | 2005-03-24 | Lg Chemical Ltd | Anion containing mixed hydroxide and lithium transition metal oxide with gradient of metal composition |
| DE10345348A1 (de) * | 2003-09-19 | 2005-04-14 | Varta Microbattery Gmbh | Verfahren zur Herstellung eines wiederaufladbaren galvanischen Elements und ein solches Element |
| DE102004008397B4 (de) * | 2004-02-20 | 2008-11-13 | Ferro Gmbh | Positives aktives Elektrodenmaterial, Verfahren zur Herstellung eines positiven aktiven Elektrodenmaterials und Lithium-Sekundärzelle |
| GB0506022D0 (en) * | 2005-03-24 | 2005-04-27 | Wildbird J C Foods Ltd | Bird feeder accessory |
| US7638243B2 (en) * | 2006-03-22 | 2009-12-29 | Novolyte Technologies Inc. | Stabilized nonaqueous electrolytes for rechargeable batteries |
| KR101151931B1 (ko) * | 2007-03-30 | 2012-06-04 | 파나소닉 주식회사 | 비수전해질 이차전지용 활물질 및 그 제조법 |
| US20080261094A1 (en) * | 2007-04-20 | 2008-10-23 | Stuart Licht | Stabilized electrodes for electrochemical cells |
| EP2228855B1 (en) | 2009-03-12 | 2014-02-26 | Belenos Clean Power Holding AG | Open porous electrically conductive nanocomposite material |
| EP2237346B1 (en) | 2009-04-01 | 2017-08-09 | The Swatch Group Research and Development Ltd. | Electrically conductive nanocomposite material comprising sacrificial nanoparticles and open porous nanocomposites produced thereof |
| CN102651491B (zh) * | 2011-02-25 | 2015-03-18 | 深圳市雄韬电源科技股份有限公司 | 一种复合电池 |
| EP3349276A3 (en) * | 2017-01-17 | 2018-09-26 | Samsung Electronics Co., Ltd. | Electrode active material, lithium secondary battery containing the electrode active material, and method of preparing the electrode active material |
| US10892488B2 (en) | 2017-01-17 | 2021-01-12 | Samsung Electronics Co., Ltd. | Electrode active material, lithium secondary battery containing the electrode active material, and method of preparing the electrode active material |
| EP3415470A1 (en) | 2017-06-14 | 2018-12-19 | Karlsruher Institut für Technologie | Boron-doped sodium-ion cathode material, method of producing same and its use |
| WO2019139443A1 (ko) | 2018-01-12 | 2019-07-18 | 한양대학교 산학협력단 | 양극활물질, 그 제조 방법, 및 이를 포함하는 리튬 이차 전지 |
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- 2000-12-01 DE DE50011303T patent/DE50011303D1/de not_active Expired - Lifetime
- 2000-12-01 WO PCT/CH2000/000641 patent/WO2001041238A1/de active IP Right Grant
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- 2000-12-01 JP JP2001542409A patent/JP2003515911A/ja active Pending
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- 2000-12-01 CN CNB008166382A patent/CN1302568C/zh not_active Expired - Fee Related
- 2000-12-01 KR KR1020027006901A patent/KR100728717B1/ko not_active IP Right Cessation
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| Publication number | Publication date |
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| US6998069B1 (en) | 2006-02-14 |
| KR20020064322A (ko) | 2002-08-07 |
| WO2001041238A1 (de) | 2001-06-07 |
| EP1236232A1 (de) | 2002-09-04 |
| JP2003515911A (ja) | 2003-05-07 |
| EP1236232B1 (de) | 2005-10-05 |
| EP1236232B8 (de) | 2005-12-07 |
| KR100728717B1 (ko) | 2007-06-14 |
| AU1506901A (en) | 2001-06-12 |
| CN1402889A (zh) | 2003-03-12 |
| DE50011303D1 (de) | 2006-02-16 |
| ATE306122T1 (de) | 2005-10-15 |
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