CN104124445B - 一种NiV3O8锂离子电池负极材料及其制备方法 - Google Patents
一种NiV3O8锂离子电池负极材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 21
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical class [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002070 nanowire Substances 0.000 claims abstract description 15
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 11
- 239000008103 glucose Substances 0.000 claims abstract description 11
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940078494 nickel acetate Drugs 0.000 claims abstract description 9
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract 2
- 239000002994 raw material Substances 0.000 claims abstract 2
- 238000000034 method Methods 0.000 abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 229910001453 nickel ion Inorganic materials 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910002986 Li4Ti5O12 Inorganic materials 0.000 description 1
- 229910032387 LiCoO2 Inorganic materials 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910005466 Ni2V2O7 Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- -1 ZnFe2O4 Chemical class 0.000 description 1
- 229910007694 ZnSnO3 Inorganic materials 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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
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- 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
- H01M4/485—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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Abstract
本发明提供一种NiV3O8锂离子电池负极材料，该锂离子电池负极材料以醋酸镍、五氧化二钒和葡萄糖为基础原料进行混合，经加水混合搅拌均匀后，转移至水热反应釜中于120‑180℃反应10‑48h，将反应所得产物在空气条件下，在300‑500℃烧结1‑10h，制得纳米线状NiV3O8锂离子电池负极材料，其纳米线长度为3‑8μm，直径为30~100 nm。本发明利用了葡萄糖的还原性将五氧化二钒还原并保持高活性，进而与镍离子结合得到中间相产物，然后利用高温烧结方法促进中间相产物继续反应。合成方法简单，易于操作，材料制备成本低。所得样品为纳米线，纳米线长度为3‑8μm，直径为30~100 nm。所制备材料容量较高，在锂离子电池中有潜在应用。
Description
技术领域
本发明涉及一种新型锂离子电池负极材料和纳米材料的制备方法，特别涉及一种三元氧化物NiV3O8纳米线锂离子电池负极材料的制备方法，属于纳米材料领域和电化学新型材料领域。
背景技术
锂离子电池是继镍镉电池、镍氢电池之后的第三代小型蓄电池，具有工作电压高，比容量高，比功率大，充放电电位曲线平稳，循环寿命长，无记忆效应，自放电小，环境友好等优点，因而广泛应用于笔记本电脑，手机等移动便携设备。不仅如此，锂离子电池也被视为是未来电动交通工具的理想电源。未来锂离子电池的研究方向主要集中在进一步提高电池的比能量及比功率，而研发高比能量、高功率锂离子电池的关键在于设计并制备出高容量、高倍率性能的电极材料。目前，正极材料一般是含锂过渡族金属氧化物（LiCoO2,LiFePO4，LiMn2O4,LiN1-y-zMnyCozOz等），现有正极材料的特点是充放电电位较高，循环性能较稳定，但比容量偏低。在现有结构基础上大幅度提高正极材料比容量的可能性并不大，进一步提高锂离子电池容量只能依赖对负极材料容量的大幅提高。传统的石墨负极材料理论容量较低，且密度较低，体积比容量低，因而研发新型高容量、高性能负极材料成为了提高锂离子电池容量的有效途径。三元化合物如 ZnFe2O4, ZnSnO3, NiSnO3, Zn2Ti3O8, Li4Ti5O12,ZnV2O4, FeVO4 等在锂离子电池中显示了潜在的应用价值，受到广泛关注。另外，材料的物理、化学性能与其形貌、结构及尺寸有十分紧密的关系。因此，发展简单方法制备具有特殊形貌和结构的新型三元化合物纳米材料并研究其电化学性能具有重要的意义。到目前为止，关于NiV3O8纳米线的制备及电化学性能研究尚未见报道。基于以上背景，本专利发明一种制备NiV3O8纳米线的新方法，以其作为锂离子电池负极显示了较好的循环性能。
发明内容
本发明的目的在于以醋酸镍、五氧化二钒、葡萄糖为前躯体，通过水热及高温烧结制备锂离子电池NiV3O8纳米线负极材料。其原理就是利用水热反应制备出中间相产物，然后利用高温加热提供反应能量，使中间相产物逐渐发生固相反应，最终得到结晶性能良好的NiV3O8纳米线。
本发明所涉及的NiV3O8合成原料为醋酸镍、五氧化二钒、葡萄糖。材料制备过程中，先将醋酸镍，五氧化二钒和葡萄糖按摩尔比2：3：1称取，放置于烧杯中加适量蒸馏水搅拌均匀，然后转移至水热反应釜中于120℃~180℃反应10~48小时。将反应产物离心、烘干，并在空气下400℃下烧结1~10小时，自然冷却可得到NiV3O8纳米线样品。
本发明所涉及的NiV3O8负极材料及制备方法具有以下几个显著的特点：
（1）本发明利用了葡萄糖的还原性将五氧化二钒还原并保持高活性，进而与镍离子结合得到中间相产物，然后利用高温烧结方法促进中间相产物继续反应。
（2）合成方法简单，易于操作，材料制备成本低。
（3）所得样品为纳米线，纳米线长度为3-8μm，直径为30~100nm。
（4）所制备材料容量较高，在锂离子电池中有潜在应用。
附图说明：
图1实施例1所制备样品的XRD图谱。
图2实施例1所制备样品的SEM图。
图3实施例1所制备样品的首次充、放电曲线(a)和循环性能图(b)。
图4实施例2所制备样品的XRD图谱。
图5实施例3所制备样品的XRD图谱。
具体实施方式：
实施例1
将醋酸镍、五氧化二钒及葡萄糖按摩尔比2：3：1称取，放置于烧杯中加适量蒸馏水搅拌均匀，转移至水热斧中在140℃下反应24小时，将反应产物离心清洗并转移至至培养皿中烘干。将烘干产物放置于石英料舟中，并将石英舟移入高温管式炉中，于400℃，空气下煅烧5小时，自然冷却可以得到NiV3O8样品。结果表明，所制备的样品经XRD图谱分析，位于15.5°, 20.4°, 21.7°, 26.2°, 31.1°, 32.4°, 33.4°, 34.3°, 41.3° 和47.5° 处的衍射峰和b-NiV3O8的 (200), (211), (012), (310), (320), (222), (500), (130), (114)和 (601) 晶面对应，与XRD 卡片JCPDS，no. 22-0455一致。所制备的样品经SEM表征，如图2(a)所示，由大量纳米线组成，纳米线长度分布为3~8 μm。由图2(b)可见，纳米线直径分布为30~100 nm。如图3所示，以所制备的NiV3O8纳米线作为锂离子电池负极材料显示其首次充、放电容量分别为839.3、1260.7 mAh/g，40次循环之后充、放电容量分别为266.3、292.9mAh/g，表明其在锂离子电池中有潜在的应用价值。
实施例2
将醋酸镍、五氧化二钒及葡萄糖按摩尔比2：3：1称取，放置于烧杯中加适量蒸馏水搅拌均匀，转移至水热斧中在140℃下反应24小时，将反应产物离心清洗并转移至至培养皿中烘干。将烘干产物放置于石英料舟中，并将石英舟移入高温管式炉中，于300℃，空气下煅烧5小时。经XRD图谱分析表明，如图4所示，所得样品为VO2。
实施例3
将醋酸镍、五氧化二钒及葡萄糖按摩尔比2：3：1称取，放置于烧杯中加适量蒸馏水搅拌均匀，转移至水热斧中在140℃下反应24小时，将反应产物离心清洗并转移至至培养皿中烘干。将烘干产物放置于石英料舟中，并将石英舟移入高温管式炉中，于500℃，空气下煅烧5小时。经XRD图谱分析表明，如图5所示，所得样品为V2O5和Ni2V2O7混合物。
Claims (1)
1.一种NiV3O8锂离子电池负极材料，其特征在于：该锂离子电池负极材料以醋酸镍、五氧化二钒和葡萄糖为基础原料制得纳米线状NiV3O8锂离子电池负极材料，其纳米线长度为3-8μm，直径为30~100 nm；
其具体的制备方法是：将醋酸镍、五氧化二钒和葡萄糖按摩尔比摩尔比2：3：1称取，加水混合搅拌均匀后，转移至水热反应釜中于120-180℃反应10-48h，将反应所得产物在空气条件下，在300-500℃烧结1-10h，制得NiV3O8锂离子电池负极材料。
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