技术领域technical field
本发明涉及锂离子电池负极材料技术领域，尤其涉及一种SiO基纳米复合材料、负极及其制备方法。The invention relates to the technical field of negative electrode materials for lithium ion batteries, in particular to a SiO-based nanocomposite material, a negative electrode and a preparation method thereof.
背景技术Background technique
锂离子电池作为目前高效储能装置之一，具有高能量密度和长循环稳定性等特点，因此被广泛的应用于电子设备和电动车辆中。然而，受到商用负极材料(石墨)的低容量限制，锂离子电池技术的能量密度达到了瓶颈，因此一系列高容量负极材料已被广泛的研究，其中具有高容量的过渡金属硫化物和硅氧基材料受到研究者的关注。As one of the current high-efficiency energy storage devices, lithium-ion batteries have the characteristics of high energy density and long cycle stability, so they are widely used in electronic equipment and electric vehicles. However, limited by the low capacity of commercial anode materials (graphite), the energy density of Li-ion battery technology has reached a bottleneck, so a series of high-capacity anode materials have been widely studied, among which transition metal sulfides and silicon oxides with high capacity Base materials have attracted the attention of researchers.
研究表明，SiO材料具有一定的循环稳定性，同时也能提供一定的容量，且绿色环保，因此以SiO材料为基体与其他材料进行复合，形成复合材料，通过物质间的相互协同作用，能保证高容量的同时提高循环稳定性。二硫化钼的理论储锂比容量约为670mAh/g，与商业化碳材料(372mAh/g)相比具有更高的理论储锂比容量，因而吸引了广泛的研究，是未来能源存储的潜力材料之一。然而这些高容量的负极材料往往遭受严重的体积效应、电子导电性差以及纳米粒子的团聚等问题，特别是纳米粒子的高表面能使得MoS2纳米片间歇地堆叠在一起，阻碍了锂离子和电子的传输。因此MoS2作为锂离子电池负极材料时具有循环稳定性和倍率性能较差等问题。Studies have shown that SiO materials have a certain cycle stability, and can also provide a certain capacity, and are environmentally friendly. Therefore, SiO materials are used as the matrix to be composited with other materials to form composite materials. Through the synergy between substances, it can ensure High capacity while improving cycle stability. The theoretical lithium storage specific capacity of molybdenum disulfide is about 670mAh/g, which is higher than that of commercial carbon materials (372mAh/g), so it has attracted extensive research and is the potential for future energy storage. one of the materials. However, these high-capacity anode materials often suffer from severe volume effects, poor electronic conductivity, and agglomeration of nanoparticles, especially the high surface energy of nanoparticles makes MoS2 nanosheets intermittently stacked together, hindering Liions and electrons transmission. Therefore, MoS2 has problems such as poor cycle stability and rate performance when used as a negative electrode material for Li-ion batteries.
如国内专利申请公开第CN108987732A号公开的一种锂离子电池SiO复合负极材料及其制备方法，该发明的制备工艺中利用二次包碳的方法制备SiO/C复合材料，先使用有机物对SiO进行碳包覆，然后再使用含氟高分子材料对SiO进行碳包覆。但是二次包碳的制备方法较为繁琐，并且复合材料的结构不易调控，使得性能一般。因此，需要寻找一种制备工艺简单、成本低廉、生产效率高、易于规模化生产、具有优异电化学性能的锂离子电池负极材料。For example, domestic patent application publication No. CN108987732A discloses a lithium ion battery SiO composite negative electrode material and its preparation method. In the preparation process of the invention, the SiO/C composite material is prepared by the method of secondary carbon coating, and the SiO is first subjected to organic matter. Carbon coating, and then carbon coating of SiO with fluorine-containing polymer material. However, the preparation method of the secondary carbon-encapsulation is cumbersome, and the structure of the composite material is not easy to control, which makes the performance general. Therefore, it is necessary to find a lithium-ion battery anode material with simple preparation process, low cost, high production efficiency, easy large-scale production, and excellent electrochemical performance.
发明内容SUMMARY OF THE INVENTION
针对现有技术中的缺点与不足，本发明的首要目的在于提供一种SiO基纳米复合材料、负极及其制备方法，基于上述目的，本发明至少提供如下技术方案：In view of the shortcomings and deficiencies in the prior art, the primary purpose of the present invention is to provide a SiO-based nanocomposite material, a negative electrode and a preparation method thereof. Based on the above purpose, the present invention provides at least the following technical solutions:
一种SiO基纳米复合材料的制备方法，其包括以下步骤：A preparation method of a SiO-based nanocomposite material, which comprises the following steps:
步骤1、取包含有纳米SiO、表面活性剂、钼酸铵以及硫脲的原料配置悬浊液；Step 1, get the raw material configuration suspension that contains nano-SiO, surfactant, ammonium molybdate and thiourea;
步骤2、将上述悬浊液置于高压水热反应釜中进行水热反应；Step 2, placing the above-mentioned suspension in a high-pressure hydrothermal reactor to carry out a hydrothermal reaction;
步骤3、收集上述水热反应获得的产物，进行沉淀物收集，以获得所述SiO基纳米复合材料的前驱体；Step 3, collecting the product obtained by the above-mentioned hydrothermal reaction, and collecting the precipitate to obtain the precursor of the SiO-based nanocomposite material;
步骤4、高温煅烧所述前驱体，以获得所述SiO基纳米复合材料。Step 4, calcining the precursor at high temperature to obtain the SiO-based nanocomposite material.
进一步的，所述步骤1包含如下子步骤：Further, the step 1 includes the following sub-steps:
取适量乙二醇及去离子水作为溶剂，将表面活性剂加入溶剂中形成溶液；Take an appropriate amount of ethylene glycol and deionized water as a solvent, and add a surfactant to the solvent to form a solution;
分别将纳米SiO、钼酸铵以及硫脲加入上述溶液中，并进行磁力搅拌形成悬浊液；Nano-SiO, ammonium molybdate and thiourea are respectively added to the above solution, and magnetic stirring is carried out to form a suspension;
其中乙二醇与去离子水的体积比为1：(3～4)。The volume ratio of ethylene glycol to deionized water is 1:(3-4).
进一步的，所述步骤1中，上述纳米SiO加入上述溶液之后进行超声处理30～60分钟，上述钼酸铵以及硫脲加入上述溶液之后进行超声处理20～40分钟，上述磁力搅拌的时间为1～2小时。Further, in the step 1, the above-mentioned nano-SiO is added to the above-mentioned solution and then subjected to ultrasonic treatment for 30 to 60 minutes, the above-mentioned ammonium molybdate and thiourea are added to the above-mentioned solution and then subjected to ultrasonic treatment for 20 to 40 minutes, and the above-mentioned magnetic stirring time is 1. ~2 hours.
进一步的，所述硫脲与所述钼酸铵的质量比为(1～1.2)：1。所述钼酸铵与所述纳米SiO的质量比为(2.5～4)：1。Further, the mass ratio of the thiourea to the ammonium molybdate is (1-1.2):1. The mass ratio of the ammonium molybdate to the nano-SiO is (2.5-4):1.
进一步的，所述表面活性剂与所述纳米SiO的质量比为(0.01～0.4)：1。Further, the mass ratio of the surfactant to the nano-SiO is (0.01-0.4):1.
进一步的，所述步骤2中，所述水热反应的条件包括：在150～200摄氏度下保温16～24小时，然后自然冷却，所述水热反应釜填料比为50％～75％。Further, in the step 2, the conditions for the hydrothermal reaction include: keeping the temperature at 150-200 degrees Celsius for 16-24 hours, and then naturally cooling, and the hydrothermal reaction kettle filling ratio is 50%-75%.
进一步的，所述步骤3中，沉淀物收集包括：将水热反应的产物离心收集后，在60～80摄氏度下真空干燥10～12小时，从而获得所述沉淀物；Further, in the step 3, the collection of the precipitate includes: after the product of the hydrothermal reaction is collected by centrifugation, vacuum-drying at 60-80 degrees Celsius for 10-12 hours, so as to obtain the precipitate;
所述步骤4中，将收集获得的上述前驱体放置于保护气体氛围中，加热至320～800摄氏度煅烧2～5小时。In the step 4, the collected precursor is placed in a protective gas atmosphere, heated to 320-800 degrees Celsius, and calcined for 2-5 hours.
进一步的，所述纳米SiO通过如下步骤获得：Further, the nano-SiO is obtained by the following steps:
取无水乙醇作为溶剂，将一氧化硅颗粒加入所述溶剂中形成悬浊液，对所述悬浊液进行真空球磨，之后进行真空干燥，以获得纳米SiO。Taking absolute ethanol as a solvent, adding silicon monoxide particles into the solvent to form a suspension, performing vacuum ball milling on the suspension, and then vacuum drying to obtain nano-SiO.
一种SiO基纳米复合材料，所述SiO基纳米复合材料包括块状纳米SiO材料，以及生长于所述块状纳米SiO材料表面的MoS2材料，所述MoS2材料呈片层结构团聚而成的类球状。A SiO-based nanocomposite material, the SiO-based nanocomposite material includes a bulk nano-SiO material, and a MoS2 material grown on the surface of the bulk nano-SiO material, and the MoS2 material is formed by agglomeration in a lamellar structure of spherical shape.
一种负极，所述负极包括所述SiO基纳米复合材料。A negative electrode comprising the SiO-based nanocomposite material.
总的说来，本发明至少具有如下有益效果：In general, the present invention at least has the following beneficial effects:
(1)本发明提供一种SiO基复合材料的制备方法，原料简单易得；合成方法较为普通，工艺简单易行，使用的仪器较为普遍，对设备要求低，成本低。(1) The present invention provides a preparation method of a SiO-based composite material, the raw materials are simple and easy to obtain; the synthesis method is relatively common, the process is simple and feasible, the used instruments are relatively common, the equipment requirements are low, and the cost is low.
(2)本发通过将纳米SiO基体与MoS2复合，制备的SiO基纳米复合材料形成了特殊的空间结构，具有一定比容量的一氧化硅与二硫化钼相结合，互为支撑，利用协同作用，在保证了复合材料高可逆容量的同时，也增加了复合材料的稳定性。片层状二硫化钼较为均匀的包覆在一氧化硅材料表面，呈现出类包覆结构，使减小二硫化钼颗粒尺寸的同时，有效的缓解了二硫化钼材料的团聚。该类包覆结构使得复合材料更加稳定，减少了不可逆容量的损失。(2) In the present invention, by compounding the nano-SiO matrix with MoS2 , the prepared SiO-based nano-composite material forms a special spatial structure, and the silicon monoxide and molybdenum disulfide with a certain specific capacity are combined to support each other and utilize synergy It also increases the stability of the composite material while ensuring the high reversible capacity of the composite material. The lamellar molybdenum disulfide is relatively uniformly coated on the surface of the silicon monoxide material, showing a quasi-coated structure, which reduces the particle size of the molybdenum disulfide and effectively relieves the agglomeration of the molybdenum disulfide material. This type of cladding structure makes the composite more stable and reduces the loss of irreversible capacity.
(3)本发明制备的SiO基纳米复合材料应用于锂离子电池负极材料时，具有循环稳定性好、倍率性能好的优点，在1000mA/g的电流密度下经过500次充放电循环之后仍可以保持450mAh/g的可逆比容量；并且在倍率性能测试中，在2A/g和4A/g的电流密度下，平均放电比容量仍然可以到达500mAh/g和430mAh/g的容量，且当电流密度恢复到100mA/g时，容量依旧可以回升,该材料用作锂离子电池负极材料呈现出了优异的电化学性能。(3) When the SiO-based nanocomposite material prepared by the present invention is applied to the negative electrode material of lithium ion battery, it has the advantages of good cycle stability and good rate performance, and can still be used after 500 charge-discharge cycles at a current density of 1000mA/g. Maintain the reversible specific capacity of 450mAh/g; and in the rate performance test, at the current density of 2A/g and 4A/g, the average discharge specific capacity can still reach the capacity of 500mAh/g and 430mAh/g, and when the current density When it is restored to 100 mA/g, the capacity can still be recovered, and the material shows excellent electrochemical performance as a negative electrode material for lithium ion batteries.
附图说明Description of drawings
图1为本发明实施例中SiO/MoS2复合材料、纳米SiO材料以及纯MoS2材料的XRD图。FIG. 1 is the XRD patterns of the SiO/MoS2 composite material, the nano-SiO material and the pure MoS2 material in the embodiment of the present invention.
图2为本发明实施例中纳米SiO材料、MoS2材料以及SiO/MoS2复合材料的SEM图。FIG. 2 is a SEM image of nano-SiO material, MoS2 material and SiO/MoS2 composite material in the embodiment of the present invention.
图3为本发明实施例中的SiO/MoS2复合材料与纯MoS2材料的交流阻抗对比图。FIG. 3 is a comparison diagram of the AC impedance of the SiO/MoS2 composite material and the pure MoS2 material in the embodiment of the present invention.
图4为本发明实施例中SiO/MoS2复合材料的循环性能曲线图(1000mAh/g)。FIG. 4 is a cycle performance curve diagram (1000mAh/g) of the SiO/MoS2 composite material in the embodiment of the present invention.
图5为本发明实施例中SiO/MoS2复合材料的倍率性能曲线图。FIG. 5 is a rate performance curve diagram of the SiO/MoS2 composite material in the embodiment of the present invention.
具体实施方式Detailed ways
下面通过附图和具体实施步骤对本发明作出进一步地详细阐述，并详细描述本发明可选择的其他实施方式。但要注意的是，本发明的具体实施步骤并不局限于目前描述的具体步骤，在不偏离本发明的实质和范围的前提下可由本领域的技术人员根据具体的实验条件和设施来实现其它的尝试。The present invention will be further elaborated below through the accompanying drawings and specific implementation steps, and other optional embodiments of the present invention will be described in detail. However, it should be noted that the specific implementation steps of the present invention are not limited to the specific steps described so far, and others can be implemented by those skilled in the art according to specific experimental conditions and facilities without departing from the spirit and scope of the present invention. attempt.
实施例Example
制备纳米SiO材料：称量质量为1～2g一氧化硅颗粒置于100ml玛瑙球磨罐中，加入研磨珠，其中研磨珠与所加入一氧化硅的质量比为(20～50):1，在球磨罐中加入20～50ml无水乙醇，在该实施例中，一氧化硅颗粒的质量优选为1～1.5g，研磨珠与所加入一氧化硅的质量比优选(40～50)：1，无水乙醇优选为30～50ml。将球磨罐转移放置进入球磨机中，设置球磨转速为200～600转每分钟，球磨时间设置为10～24小时，在该实施例中，球磨参数优选500rpm球磨10小时，真空干燥球磨产物后，得到纳米SiO材料。通过球磨法制备获得的纳米SiO产量大，过程简单易行。Preparation of nano-SiO material: weighing 1～2g of silicon monoxide particles and placing them in a 100ml agate ball mill jar, adding grinding beads, wherein the mass ratio of grinding beads to the added silicon monoxide is (20～50): 1. 20～50ml of absolute ethanol is added to the ball mill, in this embodiment, the mass of the silicon monoxide particles is preferably 1～1.5g, and the mass ratio of the grinding beads to the added silicon monoxide is preferably (40～50):1, Absolute ethanol is preferably 30 to 50 ml. The ball mill jar is transferred and placed into the ball mill, the ball milling speed is set to 200-600 rpm, and the ball-milling time is set to 10-24 hours. In this embodiment, the ball-milling parameters are preferably 500 rpm and ball-milling for 10 hours. After the ball-milling product is vacuum-dried, the obtained Nano-SiO material. The nano-SiO prepared by the ball milling method has a large yield, and the process is simple and easy to implement.
溶液配制：取体积比为1：(3～4)的乙二醇及去离子水，在该实施例中，优选体积比为1:4的乙二醇及去离子水均匀混合，作为溶剂，将十六烷基三甲基氯化铵或十六烷基三甲基季铵溴化铵作为表面活性剂加入溶剂形成溶液，将纳米SiO分散至上述溶液中，并且在室温下超声30-60分钟，优选的，在室温下超声30分钟，将钼酸铵与硫脲分散到上述溶液中，在室温超声20～40分钟后，进行约1～2小时的磁力搅拌形成悬浊液，优选的，在室温超声30分钟后，进行约1小时的磁力搅拌形成悬浊液，其中室温超声的目的是减少纳米SiO颗粒的团聚，借助乙二醇的作用使纳米SiO颗粒分散更加均匀。Solution preparation: take ethylene glycol and deionized water with a volume ratio of 1:(3～4), in this embodiment, preferably ethylene glycol and deionized water with a volume ratio of 1:4 are evenly mixed, as a solvent, Add cetyl trimethyl ammonium chloride or cetyl trimethyl quaternary ammonium bromide as a surfactant into a solvent to form a solution, disperse the nano-SiO into the above solution, and sonicate at room temperature for 30-60 minutes, preferably, 30 minutes of ultrasonic at room temperature, disperse ammonium molybdate and thiourea into the above solution, after 20 to 40 minutes of ultrasonic at room temperature, perform magnetic stirring for about 1 to 2 hours to form a suspension, preferably After 30 minutes of ultrasonic at room temperature, magnetic stirring was performed for about 1 hour to form a suspension. The purpose of ultrasonic at room temperature was to reduce the agglomeration of nano-SiO particles, and the nano-SiO particles were dispersed more uniformly with the help of ethylene glycol.
其中，纳米SiO产物与钼酸铵的质量比的选择主要是考虑到MoS2在纳米SiO表面生长的比例，使MoS2更加均匀的包覆于SiO表面；活性剂的加入使SiO颗粒表面获得更多的活性位点，促进MoS2与SiO的复合；钼酸铵与硫脲的质量比的选择主要是MoS2的化学元素比例，保证MoS2的合成。因此，上述十六烷基三甲基氯化铵或十六烷基三甲基季铵溴化铵与纳米SiO材料的质量比约为0.1～0.3:1，所述钼酸铵与纳米SiO材料的质量比为2.5～4:1，所述硫脲与钼酸铵的质量比为1～1.2:1，所述钼酸铵与溶剂的质量比为1:100。Among them, the selection of the mass ratio of nano-SiO product and ammonium molybdate is mainly to consider the growth ratio of MoS2 on the surface of nano-SiO, so that MoS2 can be more uniformly coated on the SiO surface; the addition of activator makes the surface of SiO particles more uniform There are many active sites, which promotes the composite of MoS2 and SiO; the choice of the mass ratio of ammonium molybdate and thiourea is mainly the chemical element ratio of MoS2 , which ensures the synthesis of MoS2 . Therefore, the mass ratio of the above-mentioned cetyltrimethylammonium chloride or cetyltrimethyl quaternary ammonium bromide to the nano-SiO material is about 0.1 to 0.3:1, and the ammonium molybdate to the nano-SiO material is about 0.1-0.3:1. The mass ratio of the thiourea to the ammonium molybdate is 1 to 1.2:1, and the mass ratio of the ammonium molybdate to the solvent is 1:100.
高压水热反应釜是能够分解难溶物质，其可以营造一种高温高压防腐高纯的环境发生水热反应，通过控制反应的温度、时间和溶剂来获得合成物质，得到前驱体，从而达到实验的目的，采用该方法制备SiO基纳米复合材料具有制备周期短、成本低、制备流程高效等特点。本发明选用高压水热反应釜来进行水热反应与自组装。The high-pressure hydrothermal reactor is capable of decomposing insoluble substances. It can create a high-temperature, high-pressure, anti-corrosion and high-purity environment for hydrothermal reaction. By controlling the temperature, time and solvent of the reaction, synthetic substances can be obtained, and precursors can be obtained to achieve experimental results. The purpose of this method is to prepare SiO-based nanocomposite materials with the characteristics of short preparation period, low cost, and efficient preparation process. The present invention selects a high-pressure hydrothermal reaction kettle for hydrothermal reaction and self-assembly.
水热反应：将得到的悬浊液转移到高压水热反应釜中进行水热反应，水热反应的温度设定为约180摄氏度，水热反应时间设定为约24小时。其中，高压水热反应釜的填充量约为70％。Hydrothermal reaction: transfer the obtained suspension to a high-pressure hydrothermal reaction kettle for hydrothermal reaction, the temperature of the hydrothermal reaction is set to about 180 degrees Celsius, and the hydrothermal reaction time is set to about 24 hours. Among them, the filling amount of the high-pressure hydrothermal reactor is about 70%.
沉淀收集：反应液冷却至室温，将水热反应得到的沉淀物用乙醇离心4次后在60～80摄氏度温度下真空干燥10～12小时，优选的，在80摄氏度温度下真空干燥12小时，得到SiO/MoS2复合材料前驱体。Precipitation collection: the reaction solution is cooled to room temperature, the precipitate obtained by the hydrothermal reaction is centrifuged with ethanol for 4 times, and then vacuum-dried at a temperature of 60-80 degrees Celsius for 10-12 hours, preferably, vacuum-dried at a temperature of 80 degrees Celsius for 12 hours, The SiO/MoS2 composite material precursor was obtained.
高温煅烧：将真空干燥后的SiO/MoS2复合材料前驱体在氩气氛围中煅烧3小时，煅烧温度设定为500摄氏度，得到SiO/MoS2复合材料，即SiO基纳米复合材料。High-temperature calcination: The vacuum-dried SiO/MoS2 composite material precursor was calcined in an argon atmosphere for 3 hours, and the calcination temperature was set to 500 degrees Celsius to obtain a SiO/MoS2 composite material, that is, a SiO-based nanocomposite material.
将获得的SiO基纳米复合材料依次进行调浆、涂覆以及干燥等工序之后，制备获得电极材料，以获得的电极材料作为锂离子电池负极时，可获得优异的电化学性能。After the obtained SiO-based nanocomposite material is sequentially subjected to processes such as sizing, coating and drying, an electrode material is prepared, and when the obtained electrode material is used as a negative electrode of a lithium ion battery, excellent electrochemical performance can be obtained.
图1为本发明实施例获得的SiO/MoS2复合材料、纳米SiO材料以及纯MoS2材料的XRD图，从图1中的峰值可以看出，本发明中的SiO/MoS2复合材料同时具备了SiO与MoS2两种物质的复合物相。Fig. 1 is the XRD pattern of SiO/MoS2 composite material, nano-SiO material and pure MoS2 material obtained in the embodiment of the present invention. It can be seen from the peaks in Fig. 1 that the SiO/MoS2 composite material in the present invention has both The composite phase of SiO and MoS2 was obtained.
如图2所示，其中a-b图为本发明实施例中纳米SiO材料的SEM图，由该图可以看出，纳米SiO材料呈块状结构。c-d图为本发明实施例中纯MoS2材料的SEM图，由该图可以看出，MoS2材料呈现出片层结构团聚而成的类球状。e-f图为本发明实施例中SiO/MoS2复合材料的SEM图，由该图可以得知，本发明制备的SiO/MoS2复合材料具有一包覆结构，该包覆结构主要由块状结构的纳米SiO材料，以及生长于块状结构纳米SiO材料表面的MoS2材料构成，该MoS2材料呈现出片层结构团聚而成的类球状生长于块状结构纳米SiO材料的表面。As shown in FIG. 2 , the ab diagram is the SEM image of the nano-SiO material in the embodiment of the present invention, and it can be seen from this diagram that the nano-SiO material has a block-like structure. The cd image is the SEM image of the pure MoS2 material in the embodiment of the present invention. It can be seen from this image that the MoS2 material exhibits a spherical shape formed by agglomeration of a lamellar structure. Figure ef is the SEM image of the SiO/MoS2 composite material in the embodiment of the present invention. From this figure, it can be known that the SiO/MoS2 composite material prepared by the present invention has a cladding structure, and the cladding structure is mainly composed of a block structure. The nano-SiO material and the MoS2 material grown on the surface of the bulk-structured nano-SiO material are composed of the MoS2 material showing a lamellar structure agglomerated and grown on the surface of the bulk-structured nano-SiO material.
图3为本发明实施例获得的SiO/MoS2复合材料与纯MoS2材料的交流阻抗对比图，从该图中可以看到，与纯MoS2材料相比，SiO/MoS2复合材料的内阻值小于纯MoS2材料，具有更小的物质转移电阻，由此可知，SiO/MoS2复合材料相较于纯MoS2材料具有更加优异的电化学性能。FIG.3 is a comparison diagram of the AC impedance of the SiO/MoS2 composite material obtained in the embodiment of the present invention and the pure MoS2 material. It can be seen from this figure that, compared with the pure MoS2 material, the internal The resistance value is smaller than that of pure MoS2 material, and it has smaller material transfer resistance. It can be seen that SiO/MoS2 composite material has better electrochemical performance than pure MoS2 material.
图4为以本发明实施例中的SiO/MoS2复合材料制备获得负极材料作为锂离子电池的负极时，在1000mA/g的电流密度下500次循环的充放电循环图，由该图可知，SiO/MoS2复合电极的首次库伦效率为75％，在500次循环之后该复合电极仍然可以保持450mAh/g的放电比容量，表现出稳定的循环性能。Fig. 4 is the charge-discharge cycle diagram of 500 cycles under the current density of 1000mA/g when the negative electrode material is prepared from the SiO/MoS composite material in the embodiment of the present invention and used as the negative electrode of the lithium ion battery.The first coulombic efficiency of the SiO/MoS composite electrode is 75%, and the composite electrode can still maintain a discharge specific capacity of 450 mAh/g after 500 cycles, showing stable cycling performance.
图5为以本发明实施例中的SiO/MoS2复合材料制备获得负极材料作为锂离子电池的负极时的倍率曲线，从该图中可以看出经过多次不同倍率下的充放电循环后的容量依旧可以达到初始循环标准，展现了优异的倍率性能。Fig.5 is the rate curve when the negative electrode material is prepared by using the SiO/MoS composite material in the embodiment of the present invention as the negative electrode of the lithium ion battery. The capacity can still reach the initial cycle standard, showing excellent rate performance.
由此可见，通过本发明的制备方法获得的SiO基复合材料，将具有一定比容量的一氧化硅与二氧化钼相结合，互为支撑，利用协同作用，在保证复合材料高可逆容量的同时，也增加了复合材料的稳定性。通过上述性能的测试，表明通过本发明方法获得的材料有效的缓解了二硫化钼材料的团聚，这种类包覆结构使得本发明的复合材料更加稳定，减少了不可逆容量的损失，是一种性能优异的锂离子电池负极材料。It can be seen that the SiO-based composite material obtained by the preparation method of the present invention combines silicon monoxide and molybdenum dioxide with a certain specific capacity to support each other, and utilizes the synergistic effect to ensure the high reversible capacity of the composite material at the same time. , which also increases the stability of the composite. The test of the above properties shows that the material obtained by the method of the present invention can effectively alleviate the agglomeration of the molybdenum disulfide material, and this kind of coating structure makes the composite material of the present invention more stable and reduces the loss of irreversible capacity, which is a kind of performance Excellent anode material for lithium ion batteries.
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。The above-mentioned embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations, The simplification should be equivalent replacement manners, which are all included in the protection scope of the present invention.
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| CN201910243711.4ACN110061206B (en) | 2019-03-28 | 2019-03-28 | SiO-based nano composite material, negative electrode and preparation method thereof |
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