CN114864916A - A kind of niobium pentoxide-coated graphite composite negative electrode material and preparation method thereof - Google Patents
A kind of niobium pentoxide-coated graphite composite negative electrode material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 77
- 239000010439 graphite Substances 0.000 title claims abstract description 77
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 title claims abstract description 59
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000012798 spherical particle Substances 0.000 claims abstract description 10
- 239000011247 coating layer Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000010955 niobium Substances 0.000 claims description 17
- 229910052758 niobium Inorganic materials 0.000 claims description 16
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 16
- 239000010405 anode material Substances 0.000 claims description 15
- 239000012046 mixed solvent Substances 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims description 8
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims 3
- 239000010406 cathode material Substances 0.000 claims 2
- 238000001035 drying Methods 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
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- 238000000576 coating method Methods 0.000 description 11
- 238000010586 diagram Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
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- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
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- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
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- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及电化学器件技术领域，具体涉及一种五氧化二铌包覆石墨复合负极材料及其制备方法。The invention relates to the technical field of electrochemical devices, in particular to a niobium pentoxide-coated graphite composite negative electrode material and a preparation method thereof.
背景技术Background technique
随着化石能源的过度开发、不可再生资源的日益短缺、生态环境的日渐恶化，能源危机与环境污染问题已成为人类共同关注且亟待解决的问题。因此，开发清洁、可再生的绿色新能源以及高性能储能设备已成为世界各国的研究热点。锂离子电池作为新一代绿色能量储存和转换装置，具有能量密度高、循环寿命长、放电电压高、无记忆效应、自放电率低及环境污染小等优点，已被广泛应用于便携式电子设备、大规模储能***及动力汽车等领域。然而，与传统燃油汽车相比，锂离子电池的纯电动汽车的续航里程还有一定的差距。目前，解决续航问题主要从提高电池容量和提升电池的充电速度两大方面着手。因此，开发兼具高功率密度和高能量密度的锂离子电池迫在眉睫。With the over-exploitation of fossil energy, the increasing shortage of non-renewable resources, and the deteriorating ecological environment, the energy crisis and environmental pollution have become the common concern of mankind and an urgent problem to be solved. Therefore, the development of clean and renewable green new energy and high-performance energy storage equipment has become a research hotspot around the world. As a new generation of green energy storage and conversion devices, lithium-ion batteries have the advantages of high energy density, long cycle life, high discharge voltage, no memory effect, low self-discharge rate and low environmental pollution. They have been widely used in portable electronic equipment, Large-scale energy storage systems and power vehicles and other fields. However, compared with traditional fuel vehicles, there is still a certain gap in the cruising range of pure electric vehicles with lithium-ion batteries. At present, solving the problem of battery life mainly starts from two aspects: increasing the battery capacity and increasing the charging speed of the battery. Therefore, it is urgent to develop lithium-ion batteries with high power density and high energy density.
为了解决这些问题，近年来研究人员在开发高功率密度和高能量密度的石墨负极材料方面做出了很大的努力。石墨类材料因具有优异的导电性、平稳的充放电平台、良好的锂离子嵌入-脱出能力、资源丰富、成本低廉等优点，是目前商业化应用最成功的负极材料。但随着人们对高功率和高能量密度的锂离子电池的需求越来越迫切，传统石墨负极材料面临着巨大的挑战，如快充、高安全性能、高能量密度、高功率密度等。To solve these problems, researchers have made great efforts in developing graphite anode materials with high power density and high energy density in recent years. Graphite-based materials are currently the most successful anode materials for commercial applications due to their excellent electrical conductivity, stable charge-discharge platform, good lithium ion intercalation-extraction capability, abundant resources, and low cost. However, with the increasingly urgent demand for high-power and high-energy-density Li-ion batteries, traditional graphite anode materials face huge challenges, such as fast charging, high safety performance, high energy density, and high power density.
为解决上述问题，研究人员提出了多种应对策略，主要包括改变孔隙结构、表面修饰、元素掺杂和表面包覆四种策略。其中，表面包覆被广泛用于提高其循环稳定性，其中采用氧化物材料对其表面进行包覆改性最为常见，其中最典型的就是Al2O3、SnO2、TiO2等。但是，这些金属氧化物的电子电导率较低，并不能提高石墨的快速充电能力。To solve the above problems, researchers have proposed a variety of coping strategies, including four strategies: changing the pore structure, surface modification, element doping and surface coating. Among them, surface coating is widely used to improve its cycle stability, among which the use of oxide materials to coat and modify the surface is the most common, among which the most typical ones are Al 2 O 3 , SnO 2 , TiO 2 and so on. However, the low electronic conductivity of these metal oxides does not improve the fast charging capability of graphite.
发明内容SUMMARY OF THE INVENTION
本发明的目的就是针对上述技术的不足，提供一种五氧化二铌包覆石墨复合负极材料及其制备方法，可以显著降低界面电阻，提高石墨负极材料的循环稳定性和快速充电能力，且该方法简单，成本较低，可大规模生产。The purpose of the present invention is to provide a kind of niobium pentoxide-coated graphite composite negative electrode material and its preparation method in view of the deficiencies of the above-mentioned technologies, which can significantly reduce the interface resistance, improve the cycle stability and fast charging ability of the graphite negative electrode material, and the The method is simple, the cost is low, and it can be mass-produced.
为实现上述目的，本发明所设计的一种五氧化二铌包覆石墨复合负极材料，五氧化二铌的质量占比为1～15wt%，五氧化二铌在石墨负极材料上形成均匀分布的包覆层，所述石墨负极材料为5～15μm的球形颗粒。In order to achieve the above purpose, a kind of niobium pentoxide-coated graphite composite negative electrode material designed by the present invention, the mass ratio of niobium pentoxide is 1-15wt%, and the niobium pentoxide forms a uniform distribution on the graphite negative electrode material. The coating layer, the graphite negative electrode material is spherical particles of 5-15 μm.
一种所述五氧化二铌包覆石墨复合负极材料的制备方法，包括如下步骤：A preparation method of the niobium pentoxide-coated graphite composite negative electrode material, comprising the following steps:
A）将五氯化铌溶于无水乙醇，形成铌醇溶液；A) Dissolve niobium pentachloride in absolute ethanol to form a niobium alcohol solution;
B）在所述步骤A）制得的铌醇溶液中逐滴加入去离子水，搅拌均匀，形成混合溶剂；B) adding deionized water dropwise to the niobium alcohol solution prepared in step A), stirring evenly, to form a mixed solvent;
C）向所述步骤B）制得的混合溶剂中，按照权利要求1中铌和石墨的摩尔比加入石墨，搅拌均匀，在水浴下蒸干溶剂，放入烘箱中烘干，研磨成粉末；C) In the mixed solvent prepared in the step B), add graphite according to the molar ratio of niobium and graphite in
D）将所述步骤C）制得的粉末在管式炉中进行烧结，得到五氧化二铌包覆石墨复合负极材料。D) Sintering the powder obtained in the step C) in a tube furnace to obtain a niobium pentoxide-coated graphite composite negative electrode material.
优选的，所述步骤A）中，铌醇溶液的固液质量比为1~15：155。Preferably, in the step A), the solid-liquid mass ratio of the niobium alcohol solution is 1-15:155.
优选的，所述步骤B）中，所述混合溶剂中，去离子水和无水乙醇的质量之和与五氯化铌的质量的比值为205：（1~15）。Preferably, in the step B), in the mixed solvent, the ratio of the sum of the mass of deionized water and absolute ethanol to the mass of niobium pentachloride is 205: (1~15).
优选的，所述步骤C）中，所述石墨为5～15μm的球形颗粒，水浴温度为70～80°C，水浴时搅拌速度为300～600r/min，直至蒸干溶剂为止，烘箱温度为50°C～80°C。Preferably, in the step C), the graphite is spherical particles of 5 to 15 μm, the temperature of the water bath is 70 to 80 ° C, and the stirring speed during the water bath is 300 to 600 r/min, until the solvent is evaporated to dryness, and the oven temperature is 50°C～80°C.
优选的，所述步骤D）中，所述烧结指在氩气气氛中，以2～10°C/min的升温速率至700～900°C，烧结2～3h。Preferably, in the step D), the sintering refers to sintering for 2-3 hours at a heating rate of 2-10°C/min to 700-900°C in an argon atmosphere.
本发明的原理如下：Nb2O5具有出色的倍率性能，且安全性能好，将其包覆在石墨负极材料表面，形成“核-壳”结构，既可以降低界面阻抗，提高石墨的循环稳定性和倍率性能，同时Nb2O5也可以和石墨材料协同储锂，提高其可逆容量。The principle of the invention is as follows: Nb 2 O 5 has excellent rate performance and good safety performance, and it is coated on the surface of the graphite negative electrode material to form a "core-shell" structure, which can reduce the interface impedance and improve the cycle stability of graphite At the same time, Nb 2 O 5 can also cooperate with graphite materials to store lithium and improve its reversible capacity.
本发明与现有技术相比，具有以下优点：Compared with the prior art, the present invention has the following advantages:
1、五氧化二铌包覆石墨复合负极材料具有优异的循环稳定性能；1. Niobium pentoxide-coated graphite composite anode material has excellent cycle stability;
2、在石墨材料上包覆五氧化二铌后，再烧结，形成T-五氧化二铌，可有效降低界面阻抗，提高其循环稳定性和倍率性能；2. After coating niobium pentoxide on the graphite material, it is sintered to form T-niobium pentoxide, which can effectively reduce the interface impedance and improve its cycle stability and rate performance;
3、通过简单、低成本的溶胶-凝胶法，将五氧化二铌均匀的包覆在石墨负极表面，形成均匀分布的包覆层，方法简单，成本较低，可大规模生产。3. By a simple and low-cost sol-gel method, the niobium pentoxide is uniformly coated on the surface of the graphite negative electrode to form a uniformly distributed coating layer. The method is simple, the cost is low, and it can be mass-produced.
附图说明Description of drawings
图1为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料的SEM图；Fig. 1 is the SEM image of the niobium pentoxide-coated graphite composite negative electrode material prepared in Example 3 of the present invention;
图2为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料的EDS图；Fig. 2 is the EDS figure of the niobium pentoxide-coated graphite composite negative electrode material obtained in Example 3 of the present invention;
图3为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料的XRD图；Fig. 3 is the XRD pattern of the niobium pentoxide-coated graphite composite negative electrode material prepared in Example 3 of the present invention;
图4为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料的XPS图；Fig. 4 is the XPS diagram of the niobium pentoxide-coated graphite composite negative electrode material obtained in Example 3 of the present invention;
图5为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料的电化学阻抗谱；5 is the electrochemical impedance spectrum of the niobium pentoxide-coated graphite composite negative electrode material prepared in Example 3 of the present invention;
图6为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料在0.01～3V下的循环伏安曲线；6 is the cyclic voltammetry curve of the niobium pentoxide-coated graphite composite negative electrode material prepared in Example 3 of the present invention at 0.01 to 3 V;
图7为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料组装的半电池在1C电流密度下循环200圈的容量循环图；Fig. 7 is the capacity cycle diagram of the half-cell assembled with the niobium pentoxide-coated graphite composite negative electrode material obtained in Example 3 of the present invention, which is cycled for 200 cycles at a current density of 1C;
图8为本发明中对比例1所得的Gr负极材料组装的半电池在1C电流密度下循环200圈的容量循环图；8 is a capacity cycle diagram of the half-cell assembled with the Gr negative electrode material obtained in Comparative Example 1 of the present invention cycled for 200 cycles at a current density of 1 C;
图9为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料组装的半电池在10C电流密度下循环1000圈的容量循环图；Fig. 9 is the capacity cycle diagram of the half-cell assembled with the niobium pentoxide-coated graphite composite negative electrode material obtained in Example 3 of the present invention, which is cycled for 1000 cycles at a current density of 10C;
图10为本发明中对比例1所得的Gr负极材料组装的半电池在10C电流密度下，循环1000圈的容量循环图；10 is a capacity cycle diagram of the half-cell assembled with the Gr negative electrode material obtained in Comparative Example 1 in the present invention under a current density of 10C and cycled for 1000 cycles;
图11为本发明中实施例3制得的五氧化二铌包覆石墨复合负极材料组装的半电池在不同电流密度下的倍率曲线图；Fig. 11 is the rate curve diagram of the half-cell assembled with the niobium pentoxide-coated graphite composite negative electrode material prepared in Example 3 of the present invention under different current densities;
图12为本发明中对比例1所得的Gr负极材料组装的半电池在不同电流密度下的倍率曲线图。12 is a graph showing the rate curves of the half-cell assembled with the Gr negative electrode material obtained in Comparative Example 1 of the present invention under different current densities.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明作进一步的详细说明，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments, and the technical solutions in the embodiments of the present invention will be described clearly and completely. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Example.
一种五氧化二铌包覆石墨复合负极材料，五氧化二铌的质量占比为1～15wt%，五氧化二铌在石墨负极材料上形成均匀分布的包覆层，石墨负极材料为5～15μm的球形颗粒。A niobium pentoxide-coated graphite composite negative electrode material, the mass proportion of niobium pentoxide is 1-15 wt %, the niobium pentoxide forms a uniformly distributed coating layer on the graphite negative electrode material, and the graphite negative electrode material is 5-15 wt % 15 μm spherical particles.
实施例1Example 1
A）在手套箱内，称取0.10164g（0.00037621mol）五氯化铌（相对分子质量270.17），溶解在20mL无水乙醇中，室温搅拌0.5h，形成铌醇溶液；A) In the glove box, weigh 0.10164g (0.00037621mol) of niobium pentachloride (relative molecular mass: 270.17), dissolve it in 20mL of absolute ethanol, and stir at room temperature for 0.5h to form a niobium alcohol solution;
B）在步骤A）制得的铌醇溶液中逐滴加入5ml去离子水，搅拌1h，分散均匀，形成混合溶剂；B) Add 5 ml of deionized water dropwise to the niobium alcohol solution prepared in step A), stir for 1 hour, and disperse evenly to form a mixed solvent;
C）向步骤B）制得的混合溶剂中，加入5g石墨（此包覆量为1wt%包覆，记为Gr@1-Nb2O5），石墨为5～15μm的球形颗粒，搅拌1h，分散均匀，在水浴75°C下，加热搅拌2h，搅拌速度为300r/min，直至蒸干溶剂，放入70°C烘箱中烘干，研磨成粉末；C) To the mixed solvent prepared in step B), add 5 g of graphite (the coating amount is 1 wt% coating, denoted as Gr@1-Nb 2 O 5 ), and the graphite is spherical particles of 5-15 μm, stirring for 1 h , dispersed uniformly, under 75 ℃ of water bath, heating and stirring 2h, stirring speed is 300r/min, until evaporate the solvent, put into 70 ℃ of baking ovens and dry, grind into powder;
D）将步骤C）制得的粉末在管式炉中进行烧结，在氩气气氛中，以5°C/min的升温速率至800°C，烧结2.5h，得到五氧化二铌包覆石墨复合负极材料。D) Sintering the powder obtained in step C) in a tube furnace, in an argon atmosphere, at a heating rate of 5°C/min to 800°C, sintering for 2.5h to obtain niobium pentoxide-coated graphite Composite anode material.
实施例2Example 2
A）在手套箱内，称取0.5082g（0.00188104mol）五氯化铌（相对分子质量270.17），溶解在20mL无水乙醇中，室温搅拌0.5h，形成铌醇溶液；A) In the glove box, weigh 0.5082g (0.00188104mol) of niobium pentachloride (relative molecular mass 270.17), dissolve it in 20mL of absolute ethanol, stir at room temperature for 0.5h to form a niobium alcohol solution;
B）在步骤A）制得的铌醇溶液中逐滴加入5ml去离子水，搅拌1h，分散均匀，形成混合溶剂；B) Add 5 ml of deionized water dropwise to the niobium alcohol solution prepared in step A), stir for 1 hour, and disperse evenly to form a mixed solvent;
C）向步骤B）制得的混合溶剂中，加入5g石墨（此包覆量为5wt%包覆，记为Gr@5-Nb2O5），石墨为5～15μm的球形颗粒，搅拌1h，分散均匀，在水浴70°C下，加热搅拌2h，搅拌速度为400r/min，直至蒸干溶剂，放入50°C烘箱中烘干，研磨成粉末；C) To the mixed solvent prepared in step B), add 5 g of graphite (the coating amount is 5 wt% coating, denoted as Gr@5-Nb 2 O 5 ), the graphite is spherical particles of 5-15 μm, and stir for 1 h , dispersed uniformly, under 70 ℃ of water bath, heating and stirring 2h, stirring speed is 400r/min, until evaporate the solvent, put into 50 ℃ of baking ovens and dry, grind into powder;
D）将步骤C）制得的粉末在管式炉中进行烧结，在氩气气氛中，以2°C/min的升温速率至700°C，烧结3h，得到五氧化二铌包覆石墨复合负极材料。D) Sintering the powder obtained in step C) in a tube furnace, in an argon atmosphere, at a heating rate of 2°C/min to 700°C, and sintering for 3h to obtain a niobium pentoxide-coated graphite composite negative electrode material.
实施例3Example 3
A）在手套箱内，称取1.0164g（0.00376208mol）五氯化铌（相对分子质量270.17），溶解在20mL无水乙醇中，室温搅拌0.5h，形成铌醇溶液；A) In the glove box, weigh 1.0164g (0.00376208mol) of niobium pentachloride (relative molecular mass: 270.17), dissolve it in 20mL of absolute ethanol, and stir at room temperature for 0.5h to form a niobium alcohol solution;
B）在步骤A）制得的铌醇溶液中逐滴加入5ml去离子水，搅拌1h，分散均匀，形成混合溶剂；B) Add 5 ml of deionized water dropwise to the niobium alcohol solution prepared in step A), stir for 1 hour, and disperse evenly to form a mixed solvent;
C）向步骤B）制得的混合溶剂中，加入5g石墨（此包覆量为10wt%包覆，记为Gr@10-Nb2O5），石墨为5～15μm的球形颗粒，搅拌1h，分散均匀，在水浴80°C下，加热搅拌2h，搅拌速度为600r/min，直至蒸干溶剂，放入80°C烘箱中烘干，研磨成粉末；C) To the mixed solvent prepared in step B), add 5g graphite (the coating amount is 10wt% coating, denoted as Gr@10-Nb 2 O 5 ), the graphite is spherical particles of 5-15 μm, and stir for 1h , dispersed uniformly, under 80 ℃ of water bath, heating and stirring 2h, stirring speed is 600r/min, until evaporate the solvent, put into 80 ℃ of baking ovens and dry, grind into powder;
D）将步骤C）制得的粉末在管式炉中进行烧结，在氩气气氛中，以10°C/min的升温速率至800°C，烧结3h，得到五氧化二铌包覆石墨复合负极材料。D) Sintering the powder obtained in step C) in a tube furnace, in an argon atmosphere, at a heating rate of 10°C/min to 800°C, sintering for 3h to obtain a niobium pentoxide-coated graphite composite negative electrode material.
实施例4Example 4
A）在手套箱内，称取1.5246g（0.00564311mol）五氯化铌（相对分子质量270.17），溶解在20mL无水乙醇中，室温搅拌0.5h，形成铌醇溶液；A) In the glove box, weigh 1.5246g (0.00564311mol) of niobium pentachloride (relative molecular mass 270.17), dissolve it in 20mL of absolute ethanol, stir at room temperature for 0.5h to form a niobium alcohol solution;
B）在步骤A）制得的铌醇溶液中逐滴加入5ml去离子水，搅拌1h，分散均匀，形成混合溶剂；B) Add 5 ml of deionized water dropwise to the niobium alcohol solution prepared in step A), stir for 1 hour, and disperse evenly to form a mixed solvent;
C）向步骤B）制得的混合溶剂中，加入5g石墨（此包覆量为15wt%包覆，记为Gr@15-Nb2O5），石墨为5～15μm的球形颗粒，搅拌1h，分散均匀，在水浴80°C下，加热搅拌2h，搅拌速度为600r/min，直至蒸干溶剂，放入80°C烘箱中烘干，研磨成粉末；C) To the mixed solvent prepared in step B), add 5g graphite (the coating amount is 15wt% coating, denoted as Gr@15-Nb 2 O 5 ), the graphite is spherical particles of 5-15 μm, stir for 1h , dispersed uniformly, under 80 ℃ of water bath, heating and stirring 2h, stirring speed is 600r/min, until evaporate the solvent, put into 80 ℃ of baking ovens and dry, grind into powder;
D）将步骤D）制得的粉末在管式炉中进行烧结，在氩气气氛中，以10°C/min的升温速率至900°C，烧结2h，得到五氧化二铌包覆石墨复合负极材料。D) Sintering the powder obtained in step D) in a tube furnace, in an argon atmosphere, at a heating rate of 10°C/min to 900°C, and sintering for 2h to obtain a niobium pentoxide-coated graphite composite negative electrode material.
对比例1Comparative Example 1
为未用五氧化二铌包覆处理的Gr负极材料。It is a Gr negative electrode material not coated with niobium pentoxide.
以实施例3为例，制得的五氧化二铌包覆石墨复合负极材料的SEM如图1所示，粒径约10μm，EDS如图2所示，五氧化二铌在石墨表面包覆均匀，XRD如图3所示，表明五氧化二铌为倍率性能更好的T-五氧化二铌，XPS如图4所示，五氧化二铌包覆石墨复合负极材料有Nb的峰。Taking Example 3 as an example, the SEM of the prepared niobium pentoxide-coated graphite composite anode material is shown in Figure 1, the particle size is about 10 μm, and the EDS is shown in Figure 2, and the niobium pentoxide is uniformly coated on the graphite surface. , XRD is shown in Figure 3, indicating that niobium pentoxide is T-niobium pentoxide with better rate performance, XPS is shown in Figure 4, and the niobium pentoxide-coated graphite composite anode material has a peak of Nb.
下面将实施例3制备的五氧化二铌包覆石墨复合负极材料组装成半电池，将活性材料、乙炔黑、羧甲基纤维素钠（CMC）和丁苯橡胶（SBR）以90：5：2：3的质量比混合，然后用磁力搅拌器将混合物分散在去离子水中6h以形成均匀的浆液，之后将浆料用刮刀涂布在铜箔上，最后在120°C真空烘箱干燥12h以除去水分。电极片的制作是通过将铜箔裁剪为直径10mm的圆片，裁剪后的电极片质量负载为2.5～3.5mg·cm-2，CR2016纽扣电池在氩气手套箱中进行组装。锂金属片和多孔聚丙烯膜(Celgard 2400)分别用作对电极和隔膜。电解液采用溶解于碳酸乙烯酯/碳酸甲乙酯/碳酸二甲酯 (EC/EMC/DMC)(体积比=1:1:1)中的1mol·L-1 LiPF6。Next, the niobium pentoxide-coated graphite composite negative electrode material prepared in Example 3 was assembled into a half-cell, and the active material, acetylene black, sodium carboxymethyl cellulose (CMC) and styrene-butadiene rubber (SBR) were mixed in a ratio of 90:5: The mass ratio of 2:3 was mixed, and then the mixture was dispersed in deionized water with a magnetic stirrer for 6 h to form a uniform slurry, after which the slurry was coated on copper foil with a doctor blade, and finally dried in a vacuum oven at 120 °C for 12 h. Remove moisture. The electrode sheet was fabricated by cutting the copper foil into a 10 mm diameter disc, the mass load of the cut electrode sheet was 2.5-3.5 mg·cm -2 , and the CR2016 button cell was assembled in an argon glove box. Lithium metal sheets and porous polypropylene membranes (Celgard 2400) were used as the counter electrode and separator, respectively. The electrolyte was 1 mol·L -1 LiPF 6 dissolved in ethylene carbonate/ethyl methyl carbonate/dimethyl carbonate (EC/EMC/DMC) (volume ratio=1:1:1).
如图5所示，本实施例3制备的五氧化二铌包覆石墨复合负极材料半电池的内阻大大降低。本实施例3的五氧化二铌包覆石墨复合负极材料在0.01～3V下的循环伏安曲线如图6所示，清楚地表明有五氧化二铌的氧化还原反应。As shown in FIG. 5 , the internal resistance of the half-cell of the niobium pentoxide-coated graphite composite negative electrode material prepared in Example 3 is greatly reduced. The cyclic voltammetry curve of the niobium pentoxide-coated graphite composite negative electrode material in Example 3 at 0.01-3V is shown in Figure 6, which clearly shows that there is a redox reaction of niobium pentoxide.
图7是实施例3所得的五氧化二铌包覆石墨复合负极材料组装的半电池在1C电流密度下，循环200圈的容量循环对比图，另外，图8是对比例1所得的Gr负极材料组装的半电池在1C电流密度下，循环200圈的容量循环图。FIG. 7 is a capacity cycle comparison diagram of the half-cell assembled with the niobium pentoxide-coated graphite composite negative electrode material obtained in Example 3 under a current density of 1 C and cycled for 200 cycles. In addition, FIG. 8 is the Gr negative electrode material obtained in Comparative Example 1. Capacity cycling diagram of the assembled half-cell at 1C current density for 200 cycles.
在0.01～3V，1C条件下，五氧化二铌包覆石墨复合负极材料的首次放电比容量为373.5mAh/g，循环200圈后，容量保持率可高达98.5%，而未改性的石墨的容量保持率只有53.3%。Under the conditions of 0.01-3V and 1C, the first discharge specific capacity of the niobium pentoxide-coated graphite composite anode material is 373.5mAh/g, and after 200 cycles, the capacity retention rate can be as high as 98.5%, while the unmodified graphite has a specific capacity of 373.5mAh/g. The capacity retention rate is only 53.3%.
图9是实施例3所得的五氧化二铌包覆石墨复合负极材料组装的半电池在10C电流密度下，循环1000圈的容量循环图，图10是对比例1所得的Gr负极材料组装的半电池在10C电流密度下，循环1000圈的容量循环图。Fig. 9 is the capacity cycle diagram of the half-cell assembled with the niobium pentoxide-coated graphite composite negative electrode material obtained in Example 3 under the current density of 10C and cycled for 1000 cycles, and Fig. 10 is the half-cell assembled with the Gr negative electrode material obtained in Comparative Example 1. The capacity cycling diagram of the battery cycled for 1000 cycles at a current density of 10C.
在0.01～3V，10C高倍率条件下，五氧化二铌包覆的石墨负极材料循环1000圈，仍可保留70.6mAh/g放电比容量，而未改性的石墨只有33.4mAh/g的放电比容量。Under the condition of 0.01～3V, 10C high rate, the graphite anode material coated with niobium pentoxide can still retain 70.6mAh/g discharge capacity after 1000 cycles, while the unmodified graphite has only 33.4mAh/g discharge capacity capacity.
图11是实施例3所得的五氧化二铌包覆的石墨负极材料组装的半电池在不同电流密度下的倍率曲线图，图12是对比例1所得的Gr负极材料组装的半电池在不同电流密度下的倍率曲线图，清楚地表明五氧化二铌包覆的石墨负极材料具有更好的快充性能。Fig. 11 is the rate curve diagram of the half-cell assembled with the niobium pentoxide-coated graphite negative electrode material obtained in Example 3 at different current densities, and Fig. 12 is the half-cell assembled with the Gr negative electrode material obtained in Comparative Example 1 at different currents The rate curve under density clearly shows that the niobium pentoxide-coated graphite anode material has better fast charging performance.
本发明一种五氧化二铌包覆石墨复合负极材料及其制备方法，制备的五氧化二铌包覆石墨复合负极材料具有优异的循环稳定性能，通过在石墨材料上包覆五氧化二铌后，再烧结，形成T-五氧化二铌，可有效降低界面阻抗，提高其循环稳定性和倍率性能；另外，通过简单、低成本的溶胶-凝胶法，将五氧化二铌均匀的包覆在石墨负极表面，形成均匀分布的包覆层，方法简单，成本较低，可大规模生产。The present invention is a niobium pentoxide-coated graphite composite negative electrode material and a preparation method thereof. The prepared niobium pentoxide-coated graphite composite negative electrode material has excellent cycle stability. , and then sintered to form T-niobium pentoxide, which can effectively reduce the interface impedance and improve its cycle stability and rate performance; in addition, through a simple and low-cost sol-gel method, the niobium pentoxide is uniformly coated On the surface of the graphite negative electrode, a uniformly distributed coating layer is formed, the method is simple, the cost is low, and large-scale production is possible.
在此，需要说明的是，上述技术方案的描述是示例性的，本说明书可以以不同形式来体现，并且不应被解释为限于本文阐述的技术方案。相反，提供这些说明将使得本发明公开将是彻底和完整的，并且将向本领域技术人员充分传达本说明书所公开的范围。此外，本发明的技术方案仅由权利要求的范围限定。Here, it should be noted that the descriptions of the above technical solutions are exemplary, and this specification may be embodied in different forms, and should not be construed as being limited to the technical solutions set forth herein. Rather, these descriptions are provided so that this disclosure will be thorough and complete, and will fully convey the scope of this disclosure to those skilled in the art. Furthermore, the technical solutions of the present invention are limited only by the scope of the claims.
用于描述本说明书和权利要求的各方面公开的仅仅是示例，因此，本说明书和权利要求的不限于所示出的细节。在上述描述中，当相关的已知功能或配置的详细描述被确定为不必要地模糊本说明书和权利要求的重点时，将省略详细描述。The disclosures used to describe aspects of the specification and claims are merely examples and, therefore, the description and claims are not limited to the details shown. In the above description, when a detailed description of a related known function or configuration is determined to unnecessarily obscure the gist of the specification and claims, the detailed description will be omitted.
在使用本说明书中描述的“包括”、“具有”和“包含”的情况下，除非使用否则还可以具有另一部分或其他部分，所用的术语通常可以是单数但也可以表示复数形式。Where "including", "having" and "comprising" are used as described in this specification, unless otherwise used, there may be another part or other parts, and the terms used may generally be singular but may also refer to the plural.
最后，应当指出，以上内容是结合具体实施方式对发明所做的进一步详细说明，不能认为本发明的具体实施只局限于这些说明，对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，所做出的简单替换，都应当视为属于本本发明的保护范围。以上实施例仅是本发明较有代表性的例子。显然，本发明不限于上述实施例，还可以有许多变形。凡是依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化及修饰，均应认为属于本发明的保护范围。Finally, it should be pointed out that the above content is a further detailed description of the invention in conjunction with the specific embodiments, and it should not be considered that the specific implementation of the present invention is limited to these descriptions. Under the premise of the concept of the present invention, any simple substitutions made should be regarded as belonging to the protection scope of the present invention. The above embodiments are only representative examples of the present invention. Obviously, the present invention is not limited to the above-mentioned embodiments, and many modifications are possible. Any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention shall be considered to belong to the protection scope of the present invention.
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