CN105280901B - The preparation method of spherical porous silicon carbide composite particles - Google Patents
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Abstract
本发明公开一种球形多孔硅碳复合颗粒的制备方法，包括：提供一Na2SiO3溶液；将一糖类化合物溶解于所述Na2SiO3溶液，形成一第一溶液；将所述第一溶液进行喷雾干燥，形成球形Na2SiO3/糖类复合颗粒；将所述球形Na2SiO3/糖类复合颗粒加入浓硫酸中炭化处理形成一悬浊液，进一步将上述悬浊液加入到蒸馏水中稀释并使Na2SiO3水解获得包括球形多孔SiO2/C复合颗粒的悬浊液；过滤获得球形多孔SiO2/C复合颗粒；将一还原剂与所述球形多孔SiO2/C复合颗粒混合，并加热使球形多孔SiO2/C复合颗粒中的SiO2还原，形成球形多孔Si/C复合颗粒。
The invention discloses a method for preparing spherical porous silicon-carbon composite particles, comprising: providing a Na 2 SiO 3 solution; dissolving a sugar compound in the Na 2 SiO 3 solution to form a first solution; dissolving the second A solution is spray-dried to form spherical Na 2 SiO 3 /sugar composite particles; the spherical Na 2 SiO 3 /sugar composite particles are added to concentrated sulfuric acid for carbonization to form a suspension, and the above suspension is further added to dilute in distilled water and hydrolyze Na 2 SiO 3 to obtain a suspension comprising spherical porous SiO 2 /C composite particles; filter to obtain spherical porous SiO 2 /C composite particles; mix a reducing agent with the spherical porous SiO 2 /C The composite particles are mixed and heated to reduce SiO 2 in the spherical porous SiO 2 /C composite particles to form spherical porous Si/C composite particles.
Description
技术领域technical field
本发明涉及一种球形多孔硅碳复合颗粒的制备方法。The invention relates to a method for preparing spherical porous silicon-carbon composite particles.
背景技术Background technique
锂离子电池是继铅酸电池、镍镉电池以及镍氢电池之后新一代二次电池。在全球面临石油资源的持续紧缺和环境不断恶化的今天，锂离子电池由于具有容量高、循环寿命长、自放电小、无记忆效应、无环境污染和安全性能好等优点，已经成为高新技术发展的重点之一，被认为是高容量、大功率电池的理想之选，是21世纪的环保电源。可充电锂离子电池自1990年开始商业化以来，其应用范围被不断拓展，从移动电话、笔记本电脑等便携式电子设备领域到电动汽车以及未来的航空航天、人造卫星等诸多领域都将得到广泛应用。目前，人们已经开始致力于研究新型的可充电锂离子电池，可供混合动力电动汽车、可充电混合动力车和纯电动车辆等交通工具使用，从而减少对石油的依赖和缓解空气污染。要满足这种应用，锂离子电池须具备高的功率密度、高的能量密度和好的循环性能。负极材料作为锂离子电池的重要组成部分，是锂离子储能器件发展的关键。目前商用锂离子电池负极材料主要为石墨材料，石墨具有层状结构，在充放电过程中体积膨胀小、不容易出现材料的粉化，但是石墨的理论处理容量较小，只有400mAh/g。硅由于具有最大的理论处理容量4200mAh/g而受到广泛的关注，但是由于密堆积结构，硅在充放电过程中体积膨胀大、材料粉化严重，此外纳米硅和薄膜硅制作成本高，这些都制约着其在锂离子电池中的应用。Lithium-ion batteries are a new generation of secondary batteries after lead-acid batteries, nickel-cadmium batteries and nickel-metal hydride batteries. Today, when the world is facing continuous shortage of oil resources and deteriorating environment, lithium-ion batteries have become a high-tech development due to their advantages such as high capacity, long cycle life, small self-discharge, no memory effect, no environmental pollution and good safety performance. One of the key points, it is considered to be an ideal choice for high-capacity, high-power batteries, and is an environmentally friendly power source in the 21st century. Since the commercialization of rechargeable lithium-ion batteries in 1990, its application range has been continuously expanded, ranging from portable electronic devices such as mobile phones and notebook computers to electric vehicles and future aerospace, artificial satellites and many other fields. . At present, people have begun to work on the research of new rechargeable lithium-ion batteries, which can be used in vehicles such as hybrid electric vehicles, rechargeable hybrid electric vehicles and pure electric vehicles, thereby reducing dependence on oil and alleviating air pollution. To meet this application, lithium-ion batteries must have high power density, high energy density and good cycle performance. As an important part of lithium-ion batteries, anode materials are the key to the development of lithium-ion energy storage devices. At present, the anode materials of commercial lithium-ion batteries are mainly graphite materials. Graphite has a layered structure, and its volume expansion is small during charging and discharging, and it is not easy to pulverize the material. However, the theoretical processing capacity of graphite is only 400mAh/g. Silicon has attracted widespread attention due to its maximum theoretical processing capacity of 4200mAh/g. However, due to its close-packed structure, silicon has a large volume expansion during charging and discharging, and the material is pulverized seriously. In addition, the production cost of nano-silicon and thin-film silicon is high. Restricting its application in lithium-ion batteries.
现有的硅碳复合材料可以结合上述两种材料的优点，从而获得高容量低膨胀的负极材料。然而，现有的硅碳复合材料，一般将硅粉与石墨进行简单研磨后形成，如，CN102403491A。然而，上述制备方法所获得硅碳复合材料的性能有待进一步提高。Existing silicon-carbon composite materials can combine the advantages of the above two materials to obtain high-capacity and low-expansion anode materials. However, the existing silicon-carbon composite materials are generally formed by simply grinding silicon powder and graphite, such as CN102403491A. However, the performance of the silicon-carbon composite material obtained by the above preparation method needs to be further improved.
发明内容Contents of the invention
本发明提供一种球形多孔硅碳复合颗粒的制备方法，可以解决上述问题。所述球形多孔硅碳复合颗粒的制备方法，包括如下步骤：The invention provides a method for preparing spherical porous silicon-carbon composite particles, which can solve the above problems. The preparation method of the spherical porous silicon-carbon composite particles comprises the following steps:
提供一Na2SiO3溶液；将一糖类化合物溶解于所述Na2SiO3溶液，形成一第一溶液；将所述第一溶液进行喷雾干燥，形成球形Na2SiO3/糖类复合颗粒；将所述球形Na2SiO3/糖类复合颗粒加入浓硫酸中炭化处理形成一悬浊液，所述悬浊液包括球形多孔Na2SiO3/C复合颗粒；将所述悬浊液加入蒸馏水中稀释，使球形多孔Na2SiO3/碳复合颗粒中的Na2SiO3水解，形成球形多孔SiO2/C复合颗粒；过滤获得球形多孔SiO2/C复合颗粒；将一还原剂与所述球形多孔SiO2/C复合颗粒混合，并加热使球形多孔SiO2/C复合颗粒中的SiO2还原，形成球形多孔Si/C复合颗粒。providing a Na 2 SiO 3 solution; dissolving a sugar compound in the Na 2 SiO 3 solution to form a first solution; spray-drying the first solution to form spherical Na 2 SiO 3 /sugar composite particles ; adding the spherical Na 2 SiO 3 /sugar composite particles into concentrated sulfuric acid for carbonization treatment to form a suspension, which includes spherical porous Na 2 SiO 3 /C composite particles; adding the suspension to Dilute in distilled water to hydrolyze the Na 2 SiO 3 in the spherical porous Na 2 SiO 3 /carbon composite particles to form spherical porous SiO 2 /C composite particles; filter to obtain spherical porous SiO 2 /C composite particles; mix a reducing agent with the The spherical porous SiO 2 /C composite particles are mixed and heated to reduce the SiO 2 in the spherical porous SiO 2 /C composite particles to form spherical porous Si/C composite particles.
进一步的，所述Na2SiO3溶液的浓度为15wt%到25wt%。Further, the concentration of the Na 2 SiO 3 solution is 15wt% to 25wt%.
进一步的，所述将糖类化合物溶解于所述Na2SiO3溶液的步骤包括：按照炭化率15%~25%计入硅含量5wt%~15%的糖类化合物。Further, the step of dissolving the saccharide compound in the Na 2 SiO 3 solution includes: adding the saccharide compound with a silicon content of 5wt%-15% according to a carbonization rate of 15%-25%.
进一步的，所述糖类化合物包括单糖、双糖、低聚糖和多糖。Further, the carbohydrate compounds include monosaccharides, disaccharides, oligosaccharides and polysaccharides.
进一步的，所述单糖为葡萄糖、果糖或其混合物，双糖为蔗糖、麦芽糖、乳糖或其混合物。Further, the monosaccharide is glucose, fructose or a mixture thereof, and the disaccharide is sucrose, maltose, lactose or a mixture thereof.
进一步的，所述喷雾参数为：进料量为1~10ml/min.，进口温度为100~200℃，压力为0.1~1MPa。Further, the spray parameters are as follows: feed rate is 1-10ml/min., inlet temperature is 100-200°C, and pressure is 0.1-1MPa.
进一步的，过滤获得球形多孔SiO2/C复合颗粒后，进一步包括将所述球形多孔SiO2/C复合颗粒进行清洗和干燥的步骤。Further, after the spherical porous SiO 2 /C composite particles are obtained by filtration, the step of washing and drying the spherical porous SiO 2 / C composite particles is further included.
进一步的，所述还原剂为镁粉，且所述将还原剂与所述球形多孔SiO2/C复合颗粒混合，并加热使球形多孔SiO2/C复合颗粒中的SiO2还原，形成球形多孔Si/C复合颗粒的步骤包括：将过量镁粉与所述球形多孔SiO2/C复合颗粒混合；加热使镁粉还原所述球形多孔SiO2/C复合颗粒中的SiO2，形成球形多孔Si/C复合颗粒；将上述球形多孔Si/C复合颗粒加入水中清洗；以及过滤并干燥，获得高纯度的球形多孔Si/C复合颗粒。Further, the reducing agent is magnesium powder, and the reducing agent is mixed with the spherical porous SiO 2 /C composite particles, and heated to reduce the SiO 2 in the spherical porous SiO 2 /C composite particles to form spherical porous SiO 2 The step of Si/C composite particles includes: mixing excess magnesium powder with the spherical porous SiO 2 /C composite particles; heating the magnesium powder to reduce SiO 2 in the spherical porous SiO 2 /C composite particles to form spherical porous Si /C composite particles; adding the above spherical porous Si/C composite particles into water to wash; and filtering and drying to obtain high-purity spherical porous Si/C composite particles.
进一步的，加热到600~700℃使镁粉还原所述球形多孔SiO2/C复合颗粒中的SiO2，形成球形多孔Si/C复合颗粒。Further, the magnesium powder is heated to 600-700° C. to reduce SiO 2 in the spherical porous SiO 2 /C composite particles to form spherical porous Si/C composite particles.
进一步的，所述将过量镁粉与所述球形多孔SiO2/C复合颗粒混合的步骤包括：将理论量105wt%~115wt%的镁粉与所述球形多孔SiO2/C复合颗粒混合。Further, the step of mixing excess magnesium powder with the spherical porous SiO 2 /C composite particles includes: mixing a theoretical amount of 105wt%-115wt% magnesium powder with the spherical porous SiO 2 /C composite particles.
本发明提供的一种球形多孔硅碳复合颗粒的制备方法，可以获得高纯度，微米级甚至纳米级多空Si/C复合颗粒。The invention provides a method for preparing spherical porous silicon-carbon composite particles, which can obtain high-purity, micron-scale or even nano-scale porous Si/C composite particles.
附图说明Description of drawings
图1为本发明实施例提供的球形多孔硅碳复合颗粒的制备方法流程图。Fig. 1 is a flowchart of a method for preparing spherical porous silicon-carbon composite particles provided by an embodiment of the present invention.
图2为由本实施例1得到的球形多孔硅碳复合颗粒的扫描电镜照片。FIG. 2 is a scanning electron micrograph of the spherical porous silicon-carbon composite particles obtained in Example 1. FIG.
图3为由本实施例1得到的球形多孔硅碳复合颗粒组装为扣式电池的首次循环曲线。Fig. 3 is the first cycle curve of the button battery assembled from the spherical porous silicon-carbon composite particles obtained in Example 1.
图4为由本实施例1得到的球形多孔硅碳复合颗粒组装为扣式电池的循环曲线。FIG. 4 is a cycle curve of button batteries assembled from the spherical porous silicon-carbon composite particles obtained in Example 1. FIG.
具体实施方式detailed description
下面结合附图和实施例对本发明作进一步的详细说明。可以理解的是，此处所描述的具体实施例仅仅用于解释本发明，而非对本发明的限定。另外还需要说明的是，为了便于描述，附图中仅示出了与本发明相关的部分而非全部结构。The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, but not to limit the present invention. In addition, it should be noted that, for the convenience of description, only some structures related to the present invention are shown in the drawings but not all structures.
请参照图1，一种球形多孔硅碳复合颗粒的制备方法，包括如下步骤：Please refer to Fig. 1, a kind of preparation method of spherical porous silicon-carbon composite particle, comprises the following steps:
S1，提供一Na2SiO3溶液；S1, providing a Na 2 SiO 3 solution;
S2，将一糖类化合物溶解于所述Na2SiO3溶液，形成一第一溶液；S2, dissolving a sugar compound in the Na 2 SiO 3 solution to form a first solution;
S3，将所述第一溶液进行喷雾干燥，形成球形Na2SiO3/糖类复合颗粒；S3, spray drying the first solution to form spherical Na 2 SiO 3 /sugar composite particles;
S4，将所述球形Na2SiO3/糖类复合颗粒加入浓硫酸中炭化处理形成一悬浊液，所述悬浊液包括球形多孔Na2SiO3/C复合颗粒；S4, adding the spherical Na 2 SiO 3 /sugar composite particles into concentrated sulfuric acid for carbonization to form a suspension, the suspension including spherical porous Na 2 SiO 3 /C composite particles;
S5，将所述悬浊液加入蒸馏水中稀释，使球形多孔Na2SiO3/碳复合颗粒中的Na2SiO3水解，形成球形多孔SiO2/C复合颗粒；S5, diluting the suspension into distilled water to hydrolyze the Na 2 SiO 3 in the spherical porous Na 2 SiO 3 /carbon composite particles to form spherical porous SiO 2 /C composite particles;
S6，过滤获得球形多孔SiO2/C复合颗粒；S6, obtaining spherical porous SiO 2 /C composite particles by filtration;
S7，将一还原剂与所述球形多孔SiO2/C复合颗粒混合，并加热使球形多孔SiO2/C复合颗粒中的SiO2还原，形成球形多孔Si/C复合颗粒。S7, mixing a reducing agent with the spherical porous SiO 2 /C composite particles, and heating to reduce SiO 2 in the spherical porous SiO 2 /C composite particles to form spherical porous Si/C composite particles.
在步骤S1中，所述Na2SiO3溶液的浓度为15wt%到25wt%。优选的，所述18wt%到22wt%。所述Na2SiO3溶液的浓度为20%左右。可以理解，当浓度太高，所述Na2SiO3溶液的粘度过大，不利于后续的喷雾处理；而浓度太低，不利于形成复合颗粒。In step S1, the concentration of the Na 2 SiO 3 solution is 15wt% to 25wt%. Preferably, said 18wt% to 22wt%. The concentration of the Na 2 SiO 3 solution is about 20%. It can be understood that when the concentration is too high, the viscosity of the Na 2 SiO 3 solution is too high, which is not conducive to the subsequent spraying treatment; and if the concentration is too low, it is not conducive to the formation of composite particles.
在步骤S2中，所述糖类化合物包括单糖、双糖、低聚糖和多糖。优选的，所述所述糖类化合物为单糖或双糖，这是由于单糖或双糖更有利于后续的炭化处理。进一步的，所述单糖可以为葡萄糖、果糖或其混合物。双糖可以为蔗糖、麦芽糖、乳糖或其混合物。所述糖类化合物可以按照炭化率15%~25%计入硅含量5wt%~15%加入Na2SiO3溶液中。优选的，所述糖类化合物优选的按照炭化率18%~22%计入硅含量8wt%~12%加入Na2SiO3溶液中。更优选的，所述糖类化合物优选的按照炭化率20%计入硅含量10%加入Na2SiO3溶液中。可以理解，通过加入不同量的糖类化合物可以控制最早产物中碳和硅的比例。In step S2, the carbohydrate compounds include monosaccharides, disaccharides, oligosaccharides and polysaccharides. Preferably, the saccharide compound is monosaccharide or disaccharide, because monosaccharide or disaccharide is more conducive to the subsequent carbonization treatment. Further, the monosaccharide may be glucose, fructose or a mixture thereof. The disaccharide can be sucrose, maltose, lactose or mixtures thereof. The sugar compound can be added to the Na 2 SiO 3 solution according to the carbonization rate of 15%-25% and the silicon content of 5wt%-15%. Preferably, the sugar compound is preferably added to the Na 2 SiO 3 solution according to the carbonization rate of 18%-22% and the silicon content of 8wt%-12%. More preferably, the sugar compound is preferably added to the Na 2 SiO 3 solution according to the carbonization rate of 20% and the silicon content of 10%. It is understood that the ratio of carbon to silicon in the earliest products can be controlled by adding different amounts of carbohydrate compounds.
在步骤S3中，所述喷雾参数为：进料量为1~10ml/min，进口温度为100~200℃，压力为0.1~1MPa。可以理解，通过喷雾参数的控制可以获得微米级或纳米级的球形Na2SiO3/糖类复合颗粒。优选的，所述喷雾参数为：进料量为2~5ml/min，进口温度为150~170℃，压力为0.3~0.5MPa。优选的，所述喷雾参数为：进料量为3~4ml/min，进口温度为155~160℃，压力为0.3~0.5MPa。In step S3, the spraying parameters are as follows: feed rate is 1-10ml/min, inlet temperature is 100-200°C, and pressure is 0.1-1MPa. It can be understood that micron-scale or nano-scale spherical Na 2 SiO 3 /sugar composite particles can be obtained by controlling spray parameters. Preferably, the spray parameters are as follows: feed rate is 2-5ml/min, inlet temperature is 150-170°C, and pressure is 0.3-0.5MPa. Preferably, the spray parameters are as follows: feed rate is 3-4ml/min, inlet temperature is 155-160°C, and pressure is 0.3-0.5MPa.
在步骤S4中，为了防止球形Na2SiO3/糖类复合颗粒中的Na2SiO3在空气中产生变质反应，应当将获得的球形Na2SiO3/糖类复合颗粒立即转入浓硫酸中。可以理解，球形Na2SiO3/糖类复合颗粒中的糖类化合物会经过浓硫酸脱水和炭化。进一步的，可以适当加热以促进糖类脱水反应。In step S4, in order to prevent the Na 2 SiO 3 in the spherical Na 2 SiO 3 /saccharide composite particles from deteriorating in the air, the obtained spherical Na 2 SiO 3 /saccharide composite particles should be immediately transferred to concentrated sulfuric acid . It can be understood that the sugar compounds in the spherical Na 2 SiO 3 /sugar composite particles will be dehydrated and carbonized by concentrated sulfuric acid. Further, it can be properly heated to promote the dehydration reaction of sugars.
在步骤S6中，过滤获得球形多孔SiO2/C复合颗粒后，可以进一步包括将所述球形多孔SiO2/C复合颗粒进行清洗和干燥，以去除钠离子和硫酸根等杂质。In step S6, after the spherical porous SiO 2 /C composite particles are obtained by filtration, it may further include washing and drying the spherical porous SiO 2 /C composite particles to remove impurities such as sodium ions and sulfate radicals.
在步骤S7中，所述还原剂优选的为镁粉，且所述将还原剂与所述球形多孔SiO2/C复合颗粒混合，并加热使球形多孔SiO2/C复合颗粒中的SiO2还原，形成球形多孔Si/C复合颗粒的步骤包括：In step S7, the reducing agent is preferably magnesium powder, and the reducing agent is mixed with the spherical porous SiO 2 /C composite particles, and heated to reduce the SiO 2 in the spherical porous SiO 2 /C composite particles , the steps of forming spherical porous Si/C composite particles include:
S71，将过量镁粉与所述球形多孔SiO2/C复合颗粒混合；S71, mixing excess magnesium powder with the spherical porous SiO 2 /C composite particles;
S72，加热使镁粉还原所述球形多孔SiO2/C复合颗粒中的SiO2，形成球形多孔Si/C复合颗粒；S72, heating the magnesium powder to reduce SiO 2 in the spherical porous SiO 2 /C composite particles to form spherical porous Si/C composite particles;
S73，将上述球形多孔Si/C复合颗粒加入水中清洗；以及S73, adding the above-mentioned spherical porous Si/C composite particles to water for cleaning; and
S74，过滤并干燥，获得高纯度的球形多孔Si/C复合颗粒。S74, filtering and drying to obtain high-purity spherical porous Si/C composite particles.
在步骤S71，所述将过量镁粉与所述球形多孔SiO2/C复合颗粒混合的步骤包括：将理论量105wt%~115wt%的镁粉与所述球形多孔SiO2/C复合颗粒混合。优选的，将理论量108wt%~112wt%的镁粉与所述球形多孔SiO2/C复合颗粒混合。更优选的，将理论量109wt%~111wt%的镁粉与所述球形多孔SiO2/C复合颗粒混合。将过量的镁粉与所述球形多孔SiO2/C复合颗粒反应是为了使SiO2充分还原，防止最终产物中残留SiO2。In step S71, the step of mixing excess magnesium powder with the spherical porous SiO 2 /C composite particles includes: mixing a theoretical amount of 105wt%~115wt% magnesium powder with the spherical porous SiO 2 /C composite particles. Preferably, a theoretical amount of 108wt%~112wt% magnesium powder is mixed with the spherical porous SiO 2 /C composite particles. More preferably, a theoretical amount of 109wt%~111wt% magnesium powder is mixed with the spherical porous SiO 2 /C composite particles. The purpose of reacting excess magnesium powder with the spherical porous SiO 2 /C composite particles is to fully reduce SiO 2 and prevent residual SiO 2 in the final product.
所述步骤S72优选的在惰性氛围中进行。另外，加热使镁粉还原所述SiO2的温度为600~700℃。优选的，所述加热使镁粉还原所述SiO2的温度为640~760℃。更优选的，所述加热使镁粉还原所述SiO2的温度为655~765℃。The step S72 is preferably performed in an inert atmosphere. In addition, the temperature for heating the magnesium powder to reduce the SiO2 is 600~700°C. Preferably, the temperature at which the magnesium powder reduces the SiO 2 by the heating is 640-760°C. More preferably, the temperature at which the magnesium powder reduces the SiO 2 by the heating is 655-765°C.
在步骤S73中，残余的镁粉会与水发生反应而去除，且生成的MgO也会溶解于水中而去除。In step S73, the residual magnesium powder will react with water to be removed, and the generated MgO will also be dissolved in water to be removed.
实施例1：Example 1:
配制浓度为20%的Na2SiO3溶液，按照炭化率20%计入硅含量10%的蔗糖，溶解后喷雾干燥，其中，喷雾参数为：进料量为4ml/min.，进口温度为160℃，压力为0.4MPa；获得的产物立即加入适量的浓H2SO4使蔗糖炭化，一定时间后将混合溶液缓慢加入到蒸馏水中稀释获得SiO2/C复合材料，过滤、清洗、烘干后粉末在惰性干燥气氛下与理论量110%的镁粉混合均匀、压实后在惰性气氛下600℃反应自然降温至室温后将粉末溶解于蒸馏水中使得残余的镁粉反应和生成的MgO溶解，过滤清洗、烘干后获得球形多孔Si/C复合颗粒。Prepare a Na 2 SiO 3 solution with a concentration of 20%, add sucrose with a silicon content of 10% according to the carbonization rate of 20%, and spray dry it after dissolution. The spray parameters are: the feed rate is 4ml/min., and the inlet temperature is 160 ℃, the pressure is 0.4MPa; immediately add an appropriate amount of concentrated H 2 SO 4 to the obtained product to carbonize the sucrose, and after a certain period of time, slowly add the mixed solution into distilled water to dilute to obtain a SiO 2 /C composite material, filter, wash, and dry The powder is mixed evenly with a theoretical amount of 110% magnesium powder in an inert dry atmosphere, and after compaction, it is reacted at 600°C in an inert atmosphere and naturally cooled to room temperature. After that, the powder is dissolved in distilled water to allow the residual magnesium powder to react and the generated MgO to dissolve. Spherical porous Si/C composite particles were obtained after filtering, washing and drying.
请参照图2，图2为获得的球形多孔Si/C复合颗粒的扫描电镜照片。从图中可以看出获得的球形多孔Si/C复合颗粒的最大直径为20~30微米，而最小直径可以达到100纳米左右。即，球形多孔Si/C复合颗粒的直径为30微米到100纳米。Please refer to FIG. 2 , which is a scanning electron micrograph of the obtained spherical porous Si/C composite particles. It can be seen from the figure that the maximum diameter of the obtained spherical porous Si/C composite particles is 20-30 microns, and the minimum diameter can reach about 100 nanometers. That is, the spherical porous Si/C composite particles have a diameter of 30 micrometers to 100 nanometers.
将球形多孔Si/C复合颗粒:SBR:CMC:导电剂按照质量比70:10:10:10制作成浆料，涂覆于铜箔上，烘干后组装为扣式电池测量其电化学性能。图3为扣式电池的首次循环曲线，从图中可以看出其可逆容量可达1187 mAh/g。图4为该材料的循环曲线，从图中可以看出20次循环后可逆容量还可以达到1079 mAh/g。Spherical porous Si/C composite particles: SBR: CMC: conductive agent were made into a slurry according to the mass ratio of 70:10:10:10, coated on copper foil, and assembled into a button cell after drying to measure its electrochemical performance . Figure 3 is the first cycle curve of the button battery. It can be seen from the figure that its reversible capacity can reach 1187 mAh/g. Figure 4 is the cycle curve of this material, it can be seen from the figure that the reversible capacity can reach 1079 mAh/g after 20 cycles.
注意，上述仅为本发明的较佳实施例及所运用技术原理。本领域技术人员会理解，本发明不限于这里所述的特定实施例，对本领域技术人员来说能够进行各种明显的变化、重新调整和替代而不会脱离本发明的保护范围。因此，虽然通过以上实施例对本发明进行了较为详细的说明，但是本发明不仅仅限于以上实施例，在不脱离本发明构思的情况下，还可以包括更多其他等效实施例，而本发明的范围由所附的权利要求范围决定。Note that the above are only preferred embodiments of the present invention and applied technical principles. Those skilled in the art will understand that the present invention is not limited to the specific embodiments described herein, and that various obvious changes, readjustments and substitutions can be made by those skilled in the art without departing from the protection scope of the present invention. Therefore, although the present invention has been described in detail through the above embodiments, the present invention is not limited to the above embodiments, and can also include more other equivalent embodiments without departing from the concept of the present invention, and the present invention The scope is determined by the scope of the appended claims.
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