CN106848243A - 石墨烯/氧化锡共包覆锰酸锂及其制备方法 - Google Patents
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- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 title claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 42
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910001887 tin oxide Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 4
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 8
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- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical group C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 4
- 235000011150 stannous chloride Nutrition 0.000 claims description 4
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- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 2
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 10
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- 239000003792 electrolyte Substances 0.000 description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000011572 manganese Substances 0.000 description 5
- 229910052748 manganese Inorganic materials 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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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
- H01M4/362—Composites
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
本发明涉及一种石墨烯/氧化锡共包覆锰酸锂及其制备方法,以尖晶石型锰酸锂为核,以氧化锡和石墨烯为共包覆层。本发明解决目前的包覆方法不能兼顾导电性和中和氢氟酸的缺点,该方法一步制备均匀石墨烯/氧化锡共包覆的锰酸锂材料,制备方法简单,设备条件要求低,制备的锰酸锂电化学性能优良。
Description
技术领域
本发明涉及锂电池领域,具体涉及一种石墨烯/氧化锡共包覆锰酸锂及其制备方法。
背景技术
锂离子电池具有工作电压高,能量密度大,自放电小等优点,是目前最具前景的动力电池电源体系。锰酸锂材料因为其能量密度高,安全性好,价格低廉等成为最有前途的正极材料之一。然而尖晶石型锰酸锂材料在商业化中存在的主要问题是其在循环过程中特别是高温下存在较大的容量衰减。该衰减的主要原因锰的溶解。在电解液中的氢氟酸的作用下,活性物质Mn逐渐溶蚀减少,另外电解液在锰酸锂表面的分解,也会导致界面阻抗的增大,引起材料的可逆容量衰减。
因此,对锰酸锂材料的表面改性可以成为提高锰酸锂性能的关键技术,已有大量的文献及专利证明,包覆是一种可供选择的较好的改性方法。通过包覆可以减少锰酸锂与电解液的接触,降低锰离子的溶解和电解液的氧化。如专利CN 201310362955.7中通过蒸发含铝盐的水溶液制备了铝包覆的锰酸锂,显著降低锰酸锂与电解液的接触面积,减小锰元素在电解液中的溶解,提高了循环性能和高温性能。专利CN 201210440232.X中,通过碳包覆锰酸锂,避免了高温碳化将锰酸锂晶型的破坏,同时导致金属的还原的析出。有效地提高电极导电性、改善活性材料的表面化学、保护电极避免其直接接触电解液,从而可得到更好的循环寿命。然而,现有的文献报道及专利中,通常采用碳或者氧化物单独包覆石墨烯,氧化物包覆的优点是其不但可以隔绝电解液,同时氧化物的碱性可以中和溶液中的氢氟酸,进一步减少酸对锰酸锂的侵蚀,但是氧化物通常为半导体,会降低材料的比容量。而碳材料具有很好的导电性,但是其不能和电解液中的氢氟酸发生中和反应,氢氟酸可能扩散到锰酸锂的表面,导致锰酸锂的锰的溶解。同时这些方案采用的制备工艺复杂,操作繁琐,难以大规模生产。
发明内容
本发明的目的在于提供一种石墨烯/氧化锡共包覆锰酸锂及其制备方法,解决目前的包覆方法不能兼顾导电性和中和氢氟酸的缺点,该方法一步制备均匀石墨烯/氧化锡共包覆的锰酸锂材料,制备方法简单,设备条件要求低,制备的锰酸锂电化学性能优良。
本发明所述的一种石墨烯/氧化锡共包覆锰酸锂,以尖晶石型锰酸锂为核,以氧化锡和石墨烯为共包覆层。
氧化锡的质量为锰酸锂的0.5%-5%。氧化锡的质量为包覆在锰酸锂外面的氧化锡。
所述的石墨烯/氧化锡共包覆锰酸锂的制备方法,在室温下,将氧化石墨烯分散到水,加入锰酸锂,搅拌均匀,再加入二价锡盐,过滤干燥后得到氧化锡和石墨烯共同包覆在锰酸锂。
二价锡盐为氯化亚锡或硫酸亚锡。
氧化石墨烯的质量为锰酸锂的0.5-5%。
氧化石墨烯与二价锡盐的摩尔比为0.5-5:0.5-5。
该方法一步制备均匀石墨烯/氧化锡共包覆的锰酸锂材料,由于反应产物皆能溶于水,可以通过搅拌与锰酸锂混合均匀,而反应后的产物石墨烯和二氧化锡(氧化锡)都不溶于水,沉淀在锰酸锂表面,实现石墨烯和二氧化锡均匀的覆盖的。
本发明通过在含有氧化石墨烯和锰酸锂的水溶液中加入具有还原性的二价锡盐还原石墨烯,同时本身被氧化为氧化锡,使得氧化锡和石墨烯共同包覆在锰酸锂表面。
石墨烯/氧化锡共包覆锰酸锂为锂电池正极复合材料。
与现有技术相比,本发明具有以下有益效果:
本发明石墨烯\氧化锡共包覆锰酸锂及其制备方法,解决现有包覆方法不能兼顾导电性和中和氢氟酸的缺点,该方法一步制备均匀石墨烯/氧化锡共包覆的锰酸锂材料,制备方法简单,设备条件要求低,锰酸锂和氧化锡包覆非常均匀,制备的锰酸锂电化学性能优良。
附图说明
图1包覆前的锰酸锂的SEM照片;
图2实施例1包覆后的锰酸锂的SEM照片;
图3实施例1包覆后锰酸锂常温循环性能;
图4空白锰酸锂和包覆的锰酸锂在60℃下的循环性能。
具体实施方式
下面结合实施例对本发明做进一步的说明。
实施例1
在室温下,向1000毫升水中加入0.5克氧化石墨烯,超声30分钟分散均匀,加入100克锰酸锂,搅拌30分钟,再加入3克氯化亚锡水溶液,搅拌2个小时,过滤干燥,制备得到氧化锡/石墨烯共包覆锰酸锂。
制备后的产品的SEM照片如图2,从图2可以看出,石墨烯和白色的氧化锡均匀的包覆在锰酸锂表面。
实施例2
在室温下,向1000毫升水中加入5克氧化石墨烯,超声40分钟分散均匀,加入100克锰酸锂,搅拌50分钟,再加入0.5克氯化亚锡水溶液,搅拌3个小时,过滤干燥,制备得到氧化锡/石墨烯共包覆锰酸锂。
实施例3
在室温下,向1000毫升水中加入2克氧化石墨烯,超声40分钟分散均匀,加入100克锰酸锂,搅拌20分钟,再加入1克硫酸化亚锡水溶液,搅拌1个小时,过滤干燥,制备得到氧化锡/石墨烯共包覆锰酸锂。
图1为未包覆锰酸锂的SEM照片。
将实施例1最终所得产物以8:1:1质量比与炭黑,PVDF相混合,NMP做溶剂充分搅拌,混合均匀后涂至铝箔,在100℃条件下真空干燥12h。裁片后,在手套箱中以锂片为负极组装成电池,并在充放电仪做高倍率性能测试。图3为实施例1包覆后锰酸锂常温循环性能。图4为实施例1包覆和未包覆的锰酸锂在60℃下的循环性能。
从图可以发现,所制备锰酸锂电化学性能优良,常温1C条件下容量可达106mAh/g,循环300周容量几乎没有衰减,高温下循环280周后容量保持率依旧有85%,而未包覆的锰酸锂循环50周后容量只有30%。
上述虽然对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,所属领域技术人员应该明白,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。
Claims (6)
1.一种石墨烯/氧化锡共包覆锰酸锂,其特征在于,以尖晶石型锰酸锂为核,以氧化锡和石墨烯为共包覆层。
2.根据权利要求1所述的石墨烯/氧化锡共包覆锰酸锂,其特征在于,氧化锡的质量为锰酸锂的0.5%-5%。
3.一种权利要求1所述的石墨烯/氧化锡共包覆锰酸锂的制备方法,其特征在于,在室温下,将氧化石墨烯分散到水,加入锰酸锂,搅拌均匀,再加入二价锡盐,过滤干燥后得到氧化锡和石墨烯共同包覆在锰酸锂。
4.根据权利要求3所述的石墨烯/氧化锡共包覆锰酸锂的制备方法,其特征在于,二价锡盐为氯化亚锡或硫酸亚锡。
5.根据权利要求3所述的石墨烯/氧化锡共包覆锰酸锂的制备方法,其特征在于,氧化石墨烯的质量为锰酸锂的0.5-5%。
6.根据权利要求3所述的石墨烯/氧化锡共包覆锰酸锂的制备方法,其特征在于,氧化石墨烯与二价锡盐的摩尔比为0.5-5:0.5-5。
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CN111193007A (zh) * | 2020-02-28 | 2020-05-22 | 浙江克能新能源科技有限公司 | 一种锰酸锂材料电池的正极和制备方法以及锰酸锂电池 |
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CN110563052A (zh) * | 2019-09-09 | 2019-12-13 | 河北省科学院能源研究所 | 一种碳和氧化镧共包覆改性镍锰酸锂正极材料的制备方法 |
CN110563052B (zh) * | 2019-09-09 | 2021-11-05 | 河北省科学院能源研究所 | 一种碳和氧化镧共包覆改性镍锰酸锂正极材料的制备方法 |
CN111193007A (zh) * | 2020-02-28 | 2020-05-22 | 浙江克能新能源科技有限公司 | 一种锰酸锂材料电池的正极和制备方法以及锰酸锂电池 |
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