CN108470891A - The method for preparing silicon-carbon cathode material based on micron silica - Google Patents
The method for preparing silicon-carbon cathode material based on micron silica Download PDFInfo
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Abstract
基于微米二氧化硅制备硅碳负极材料的方法，步骤为：1)按SiO2：碳源：水＝(30～80)：(5～15)：(60～120)的质量比，配成浆液，湿法研磨4～5h，冷冻干燥得到纳米级的SiO2；2)将1)所得物高温碳化，得SiO2@C材料，再按照SiO2@C：Mg：NaCl质量比1:1:1～1:1:10的比例，在600～750℃下镁热还原，之后酸洗、洗涤、干燥得Si@C纳米颗粒；3)将2)的纳米颗粒与氧化石墨烯溶液超声混匀，喷雾热裂解包覆还原，制得材料。本发明成本低廉，操作简单，不易团聚，可以维持样品原貌，产品结构稳定性好，材料的导电性和离子传输能力强。
The method for preparing a silicon-carbon negative electrode material based on micron silica, the steps are: 1) According to the mass ratio of SiO 2 : carbon source: water = (30-80): (5-15): (60-120), formulate Slurry, wet grinding for 4-5 hours, freeze-drying to obtain nano-scale SiO 2 ; 2) high-temperature carbonization of the obtained product in 1) to obtain SiO 2 @C material, and then according to SiO 2 @C:Mg:NaCl mass ratio 1:1 : ratio of 1 to 1:1:10, magnesia thermal reduction at 600 to 750°C, pickling, washing, and drying to obtain Si@C nanoparticles; 3) Ultrasonic mixing of the nanoparticles in 2) with the graphene oxide solution uniform, spray pyrolysis coating reduction, and obtain the material. The invention has low cost, simple operation, is not easy to agglomerate, can maintain the original appearance of the sample, has good product structure stability, and has strong electrical conductivity and ion transmission capacity of the material.
Description
技术领域technical field
本发明属于硅碳负极材料制备领域，具体涉及一种基于微米二氧化硅制备硅碳负极材料的方法。The invention belongs to the field of preparation of silicon-carbon negative electrode materials, and in particular relates to a method for preparing silicon-carbon negative electrode materials based on micron silicon dioxide.
背景技术Background technique
硅基材料是非常具有潜力的高性能锂离子电池负极材料，具有迄今已知最高的理论比容量(4200mAh/g)和较低的嵌锂电位(0.1Vvs.Li/Li+)，并且资源丰富，环境友好。但是硅负极在脱嵌锂过程中伴随巨大的体积变化(高达300％)，会导致硅颗粒破碎、粉化，使电极材料失去电活性，表现为极差的循环稳定性；此外，硅本身的电导率不高，倍率特性较差，这严重影响了硅材料作为锂离子电池负极材料的应用。硅碳复合材料作为缓解上述问题的有效途径，得到了广泛的研究。于晓磊(锂离子电池用高性能硅碳复合负极材料的制备与性能研究，上海交通大学硕士论文，2013)利用纳米硅粉和介孔二氧化硅(SBA-15)两种不同的硅源，制备了球形多孔的硅/石墨烯@碳(Si/GNS@C)复合材料，但是其中的包碳方法为化学气相沉积法，该方法不易工业化推广应用；陶华超等人(镁热还原法制备多孔硅碳复合负极材料，《硅酸盐学报》2013年08期)以介孔SiO2为硅源直接镁热还原制备得到硅碳材料，由于纳米级SiO2的制备大多依赖生物质硅源或者正硅酸乙酯(TEOS)水解制得，且形成的颗粒容易团聚，导致制备成本高，镁热反应效果不理想。Silicon-based materials are very potential high-performance lithium-ion battery anode materials, with the highest known theoretical specific capacity (4200mAh/g) and low lithium intercalation potential (0.1Vvs.Li/Li+), and abundant resources. Environment friendly. However, the silicon negative electrode is accompanied by a huge volume change (up to 300%) during the process of deintercalating lithium, which will cause the silicon particles to be broken and pulverized, and the electrode material will lose its electrical activity, showing extremely poor cycle stability; in addition, the silicon itself The conductivity is not high and the rate characteristics are poor, which seriously affects the application of silicon materials as anode materials for lithium-ion batteries. Silicon-carbon composites have been extensively studied as an effective way to alleviate the above problems. Yu Xiaolei (Preparation and Performance Research of High-performance Silicon-Carbon Composite Anode Materials for Lithium-ion Batteries, Master Thesis of Shanghai Jiao Tong University, 2013) using two different silicon sources of nano-silica powder and mesoporous silica (SBA-15) , prepared a spherical porous silicon/graphene@carbon (Si/GNS@C) composite material, but the carbon coating method is chemical vapor deposition, which is not easy to be popularized and applied in industrialization; Tao Huachao et al. (prepared by magnesia thermal reduction method Porous silicon-carbon composite anode material, "Journal of China Ceramics" 2013 08) SiC materials were prepared by direct magnesia thermal reduction of mesoporous SiO 2 as silicon source, since the preparation of nano-scale SiO 2 mostly relies on biomass silicon source or It is produced by hydrolysis of orthoethyl silicate (TEOS), and the formed particles are easy to agglomerate, resulting in high preparation cost and unsatisfactory magnesium thermal reaction effect.
发明内容Contents of the invention
为了克服现有技术的不足，本发明提供了基于微米二氧化硅制备硅碳负极材料的方法，具有成本低、易工业化生产，制备的产品体积膨胀小、导电性强的优点。In order to overcome the deficiencies of the prior art, the present invention provides a method for preparing a silicon-carbon negative electrode material based on micron silicon dioxide, which has the advantages of low cost, easy industrial production, small volume expansion of the prepared product, and strong conductivity.
为了达到上述目的，本发明采取的技术方案为：In order to achieve the above object, the technical scheme that the present invention takes is:
基于微米二氧化硅制备硅碳负极材料的方法，包括以下步骤：The method for preparing a silicon-carbon negative electrode material based on micron silicon dioxide comprises the following steps:
步骤一：按照二氧化硅：碳源：水＝(30～80)：(5～15)：(60～120)的质量比，分别量取粒径50～100um的二氧化硅、碳源和水配制成浆液，利用砂磨机湿法研磨4～5h，再冷冻干燥得到纳米级的SiO2；Step 1: Measure silicon dioxide, carbon source and Water is prepared into a slurry, wet-grinded with a sand mill for 4-5 hours, and then freeze-dried to obtain nano-sized SiO 2 ;
步骤二：将步骤一所得物进行高温碳化，得到SiO2@C材料，然后按照SiO2@C：Mg：NaCl质量比为1:1:1～1:1:10的比例，在600～750℃条件下镁热还原，之后酸洗、洗涤、干燥制得Si@C纳米颗粒；Step 2: Carry out high-temperature carbonization on the product obtained in Step 1 to obtain SiO 2 @C material, and then according to the ratio of SiO 2 @C:Mg:NaCl mass ratio of 1:1:1～1:1:10, at 600～750 Magnesium thermal reduction at ℃, followed by pickling, washing, and drying to obtain Si@C nanoparticles;
步骤三：将步骤二制得的Si@C纳米颗粒与氧化石墨烯溶液超声混匀后，通过喷雾热裂解技术进行包覆还原，制得Si@C@G材料。Step 3: After ultrasonically mixing the Si@C nanoparticles prepared in Step 2 with the graphene oxide solution, the spray pyrolysis technology is used for coating and reduction to prepare the Si@C@G material.
进一步的，所述碳源为葡萄糖、酚醛树脂、聚乙烯吡咯烷酮、聚丙烯腈之一。Further, the carbon source is one of glucose, phenolic resin, polyvinylpyrrolidone, and polyacrylonitrile.
进一步的，步骤一冷冻干燥的温度为-45℃。Further, the freeze-drying temperature in the first step is -45°C.
进一步的，步骤二的高温碳化在450～700℃下进行，碳化2～4h。Further, the high-temperature carbonization in step 2 is carried out at 450-700° C., and the carbonization takes 2-4 hours.
进一步的，步骤二所述的酸洗、洗涤过程为：利用2mol/L盐酸酸洗除去杂质，再用5％的氢氟酸洗涤30min，除去未反应的SiO2，最后再用去离子水、乙醇洗涤至中性。Further, the pickling and washing process described in step 2 is: pickling with 2 mol/L hydrochloric acid to remove impurities, then washing with 5% hydrofluoric acid for 30 minutes to remove unreacted SiO 2 , and finally using deionized water, Wash with ethanol until neutral.
进一步的，步骤三所述的包覆还原的过程为：利用超声形成喷雾，实现造粒功能，再将制得的球状颗粒以H2/Ar混合气为载气，通入600～800℃的立式管式炉进行包覆还原作业，最后通过静电场收集得到干燥的Si@C@G材料。Further, the coating reduction process described in Step 3 is: use ultrasonic to form a spray to realize the granulation function, and then use the H 2 /Ar mixed gas as the carrier gas to pass the prepared spherical particles into a 600-800 ° C The vertical tube furnace is used for coating reduction operation, and finally the dry Si@C@G material is collected by electrostatic field.
本发明的有益效果：Beneficial effects of the present invention:
本发明利用微米级SiO2为原料，通过湿法研磨制备材料，成本低廉，操作简单，还能克服依赖生物质硅源或者正硅酸乙酯TEOS水解制得的纳米级的SiO2容易团聚、导致制备成本高、后期镁热反应效果不理想的问题；而通过冷冻干燥技术，可以维持样品原貌，更具有商业化前景。The present invention uses micron-sized SiO2 as raw material and prepares materials by wet grinding, which has low cost and simple operation, and can also overcome the difficulty of agglomeration and easy agglomeration of nano-sized SiO2 obtained by hydrolyzing biomass silicon or tetraethylorthosilicate TEOS. It leads to the problems of high preparation cost and unsatisfactory effect of magnesium thermal reaction in the later stage; and through freeze-drying technology, the original appearance of the sample can be maintained, which has more commercial prospects.
选取有机高分子碳源，碳化后可得到三维多孔结构包覆的多孔SiO2@C材料，通过控制助熔剂NaCl的量，控制SiC的生成，有利于充放电过程中的维持材料的结构稳定性，同时，高分子碳源有助于缓冲体积膨胀。Select an organic polymer carbon source, and after carbonization, a porous SiO 2 @C material coated with a three-dimensional porous structure can be obtained. By controlling the amount of flux NaCl, the generation of SiC is controlled, which is conducive to maintaining the structural stability of the material during the charging and discharging process. , at the same time, the polymer carbon source helps to buffer the volume expansion.
利用喷雾热裂解将Si@C与石墨烯复合，进行二次包覆。在超声喷雾过程中，可以有效的实现造粒功能，得到颗粒均匀的球状颗粒；而氧化石墨烯在载气Ar/H2气体的还原作用下，生成石墨烯，包覆在Si@C材料表面，增强材料的导电性和离子传输能力，更好的改善硅基材料导电性能差的劣势，得到性能优良的硅碳复合材料。 Si@C and graphene were composited by spray pyrolysis for secondary coating. In the ultrasonic spraying process, the granulation function can be effectively realized, and spherical particles with uniform particles can be obtained; while the graphene oxide is reduced by the carrier gas Ar/H 2 gas to generate graphene, which is coated on the surface of the Si@C material. , enhance the electrical conductivity and ion transport capacity of the material, better improve the disadvantage of poor electrical conductivity of the silicon-based material, and obtain a silicon-carbon composite material with excellent performance.
附图说明Description of drawings
图1是砂磨后的粒径分布图；Fig. 1 is the particle size distribution figure after sanding;
图2是不同NaCl添加量下镁热后的X射线衍射图；Fig. 2 is the X-ray diffraction pattern after magnesium heating under different NaCl additions;
图3是Si@C喷雾干燥后的粒径放大图。Figure 3 is an enlarged view of the particle size of Si@C after spray drying.
具体实施方式Detailed ways
下面结合具体实施例对本发明做进一步说明。The present invention will be further described below in conjunction with specific embodiments.
实施例1Example 1
称取SiO2 30g，聚乙烯吡咯烷酮5g以及水120mL于砂磨机中，湿法研磨4h，分离后，置于冰箱冷冻，在冷干机里中-45℃条件下冷冻干燥两天两夜。Weigh 30g of SiO 2 , 5g of polyvinylpyrrolidone and 120mL of water in a sand mill, wet grind for 4 hours, separate, freeze in the refrigerator, and freeze-dry in a freeze dryer at -45°C for two days and two nights.
将冷干后的产物置于管式炉中，在惰性气氛里450℃条件下煅烧4h，得到SiO2@C材料，然后按照SiO2@C:Mg:NaCl的质量比为1:1:1的比例，在惰性气氛中，650℃条件下镁热还原4h，在2M的盐酸溶液里洗涤8h，除去镁热反应副产物；将酸洗后的溶液加入质量分数为5％的氢氟酸溶液中洗涤0.5h，除去未完全反应的SiO2，用去离子水和乙醇溶液洗涤，过滤至中性后，置于真空烘箱中，80℃条件下真空干燥12h，得到Si@C复合材料。The freeze-dried product was placed in a tube furnace and calcined at 450°C for 4 hours in an inert atmosphere to obtain a SiO 2 @C material, and then the mass ratio of SiO 2 @C:Mg:NaCl was 1:1:1 In an inert atmosphere, magnesia thermal reduction at 650°C for 4 hours, washing in 2M hydrochloric acid solution for 8 hours, to remove magnesia thermal reaction by-products; add the solution after pickling to 5% hydrofluoric acid solution Wash for 0.5 h to remove incompletely reacted SiO 2 , wash with deionized water and ethanol solution, filter to neutral, place in a vacuum oven, and vacuum dry at 80°C for 12 h to obtain a Si@C composite material.
将Si@C复合材料和氧化石墨烯按照质量比为10:1称取，加入到20mL水中，超声15min，使之充分分散在水溶液中。利用喷雾热裂解装置，将混合液喷雾到管式炉中，在800℃的H2/Ar混合载气的还原作用下，还原制得Si@C@G颗粒，通过静电场作用进行收集。The Si@C composite material and graphene oxide were weighed according to a mass ratio of 10:1, added to 20 mL of water, and ultrasonicated for 15 min to fully disperse them in the aqueous solution. Using a spray pyrolysis device, the mixed solution was sprayed into a tube furnace, and under the reducing action of H2 / Ar mixed carrier gas at 800 °C, Si@C@G particles were reduced to obtain Si@C@G particles, which were collected by electrostatic field.
实施例2Example 2
称取SiO2 40g，聚乙烯吡咯烷酮10g以及水120mL与砂磨机中，湿法研磨4h，分离后，置于冰箱冷冻，在冷干机里中-45℃条件下冷冻干燥两天两夜。Weigh 40g of SiO 2 , 10g of polyvinylpyrrolidone and 120mL of water into a sand mill, wet grind for 4 hours, separate, freeze in the refrigerator, and freeze-dry in a freeze dryer at -45°C for two days and two nights.
将冷干后的产物置于管式炉中，在惰性气氛里450℃条件下煅烧4h，得到SiO2@C材料，然后按照SiO2@C:Mg:NaCl的质量比为1:1:1的比例，在惰性气氛中，650℃条件下镁热还原4h，在2M的盐酸溶液里洗涤8h，除去镁热反应副产物；将酸洗后的溶液加入质量分数为5％的氢氟酸溶液中洗涤0.5h，除去未完全反应的SiO2，用去离子水和乙醇溶液洗涤，过滤至中性后，置于真空烘箱中，80℃条件下真空干燥12h，得到Si@C复合材料。The freeze-dried product was placed in a tube furnace and calcined at 450°C for 4 hours in an inert atmosphere to obtain a SiO 2 @C material, and then the mass ratio of SiO 2 @C:Mg:NaCl was 1:1:1 In an inert atmosphere, magnesia thermal reduction at 650°C for 4 hours, washing in 2M hydrochloric acid solution for 8 hours, to remove magnesia thermal reaction by-products; add the solution after pickling to 5% hydrofluoric acid solution Wash for 0.5 h to remove incompletely reacted SiO 2 , wash with deionized water and ethanol solution, filter to neutral, place in a vacuum oven, and vacuum dry at 80°C for 12 h to obtain a Si@C composite material.
将Si@C复合材料和氧化石墨烯按照质量比为10:1称取，加入到20mL水中，超声15min，使之充分分散在水溶液中。利用喷雾热裂解装置，将混合液喷雾到管式炉中，在800℃的H2/Ar混合载气的还原作用下，还原制得Si@C@G颗粒，通过静电场作用进行收集。The Si@C composite material and graphene oxide were weighed according to a mass ratio of 10:1, added to 20 mL of water, and ultrasonicated for 15 min to fully disperse them in the aqueous solution. Using a spray pyrolysis device, the mixed solution was sprayed into a tube furnace, and under the reducing action of H 2 /Ar mixed carrier gas at 800°C, Si@C@G particles were reduced to obtain Si@C@G particles, which were collected by electrostatic field.
实施例3Example 3
称取SiO2 60g，聚乙烯吡咯烷酮5g以及水120mL与砂磨机中，湿法研磨4h，分离后，置于冰箱冷冻，在冷干机里中-45℃条件下冷冻干燥两天两夜。Weigh 60g of SiO 2 , 5g of polyvinylpyrrolidone and 120mL of water into a sand mill, wet grind for 4 hours, separate, freeze in the refrigerator, and freeze-dry in a freeze dryer at -45°C for two days and two nights.
将冷干后的产物置于管式炉中，在惰性气氛里500℃条件下煅烧4h，得到SiO2@C材料，然后按照SiO2@C：Mg：NaCl的质量比为1:1:3的比例，在惰性气氛中，650℃条件下镁热还原4h，在2M的盐酸溶液里洗涤8h，除去镁热反应副产物；将酸洗后的溶液加入质量分数为5％的氢氟酸溶液中洗涤0.5h，除去未完全反应的SiO2，用去离子水和乙醇溶液洗涤，过滤至中性后，置于真空烘箱中，80℃条件下真空干燥12h，得到Si@C复合材料。The freeze-dried product was placed in a tube furnace and calcined at 500°C for 4 hours in an inert atmosphere to obtain a SiO 2 @C material, and then the SiO 2 @C:Mg:NaCl mass ratio was 1:1:3 In an inert atmosphere, magnesia thermal reduction at 650°C for 4 hours, washing in 2M hydrochloric acid solution for 8 hours, to remove magnesia thermal reaction by-products; add the solution after pickling to 5% hydrofluoric acid solution Wash for 0.5 h to remove incompletely reacted SiO 2 , wash with deionized water and ethanol solution, filter to neutral, place in a vacuum oven, and vacuum dry at 80°C for 12 h to obtain a Si@C composite material.
将Si@C复合材料和氧化石墨烯按照质量比为10:1称取，加入到20mL水中，超声15min，使之充分分散在水溶液中。利用喷雾热裂解装置，将混合液喷雾到管式炉中，在800℃的H2/Ar混合载气的还原作用下，还原制得Si@C@G颗粒，通过静电场作用进行收集。The Si@C composite material and graphene oxide were weighed according to a mass ratio of 10:1, added to 20 mL of water, and ultrasonicated for 15 min to fully disperse them in the aqueous solution. Using a spray pyrolysis device, the mixed solution was sprayed into a tube furnace, and under the reducing action of H2/Ar mixed carrier gas at 800 °C, the Si@C@G particles were reduced to obtain Si@C@G particles, which were collected by electrostatic field.
实施例4Example 4
称取SiO2 80g，聚乙烯吡咯烷酮5g以及水100mL与砂磨机中，湿法研磨5h，分离后，置于冰箱冷冻，在冷干机里中-45℃条件下冷冻干燥两天两夜。Weigh 80g of SiO 2 , 5g of polyvinylpyrrolidone and 100mL of water into a sand mill, wet grind for 5h, separate, freeze in the refrigerator, and freeze-dry in a freeze dryer at -45°C for two days and two nights.
将冷干后的产物置于管式炉中，在惰性气氛里500℃条件下煅烧3h，得到SiO2@C材料，然后按照SiO2@C：Mg：NaCl的质量比为1:1:5的比例，在惰性气氛中，700℃条件下镁热还原4h，在2M的盐酸溶液里洗涤8h，除去镁热反应副产物；将酸洗后的溶液加入质量分数为5％的氢氟酸溶液中洗涤0.5h，除去未完全反应的SiO2，用去离子水和乙醇溶液洗涤，过滤至中性后，置于真空烘箱中，80℃条件下真空干燥12h，得到Si@C复合材料。The freeze-dried product was placed in a tube furnace, and calcined at 500°C for 3 hours in an inert atmosphere to obtain a SiO 2 @C material, and then the SiO 2 @C:Mg:NaCl mass ratio was 1:1:5 In an inert atmosphere, magnesia thermal reduction at 700°C for 4 hours, washing in 2M hydrochloric acid solution for 8 hours, to remove magnesia thermal reaction by-products; add the solution after pickling to 5% hydrofluoric acid solution Wash for 0.5 h to remove incompletely reacted SiO 2 , wash with deionized water and ethanol solution, filter to neutral, place in a vacuum oven, and vacuum dry at 80°C for 12 h to obtain a Si@C composite material.
将Si@C复合材料和氧化石墨烯按照质量比为10:1称取，加入到20mL水中，超声15min，使之充分分散在水溶液中。利用喷雾热裂解装置，将混合液喷雾到管式炉中，在800℃的H2/Ar混合载气的还原作用下，还原制得Si@C@G颗粒，通过静电场作用进行收集。The Si@C composite material and graphene oxide were weighed according to a mass ratio of 10:1, added to 20 mL of water, and ultrasonicated for 15 min to fully disperse them in the aqueous solution. Using a spray pyrolysis device, the mixed solution was sprayed into a tube furnace, and under the reducing action of H 2 /Ar mixed carrier gas at 800°C, Si@C@G particles were reduced to obtain Si@C@G particles, which were collected by electrostatic field.
实施例5Example 5
称取SiO2 60g，聚乙烯吡咯烷酮5g以及水100mL与砂磨机中，湿法研磨4h，分离后，置于冰箱冷冻，在冷干机里中-45℃条件下冷冻干燥两天两夜。Weigh 60g of SiO 2 , 5g of polyvinylpyrrolidone and 100mL of water into a sand mill, wet grind for 4 hours, separate, freeze in the refrigerator, and freeze-dry in a freeze dryer at -45°C for two days and two nights.
将冷干后的产物置于管式炉中，在惰性气氛里450℃条件下煅烧4h，得到SiO2@C材料，然后按照SiO2@C：Mg：NaCl的质量比为1:1:10的比例，在惰性气氛中，700℃条件下镁热还原4h，在2M的盐酸溶液里洗涤8h，除去镁热反应副产物；将酸洗后的溶液加入质量分数为5％的氢氟酸溶液中洗涤0.5h，除去未完全反应的SiO2，用去离子水和乙醇溶液洗涤，过滤至中性后，置于真空烘箱中，80℃条件下真空干燥12h，得到Si@C复合材料。The freeze-dried product was placed in a tube furnace and calcined at 450°C for 4 hours in an inert atmosphere to obtain a SiO 2 @C material, and then the mass ratio of SiO 2 @C:Mg:NaCl was 1:1:10 In an inert atmosphere, magnesia thermal reduction at 700°C for 4 hours, washing in 2M hydrochloric acid solution for 8 hours, to remove magnesia thermal reaction by-products; add the solution after pickling to 5% hydrofluoric acid solution Wash for 0.5 h to remove incompletely reacted SiO 2 , wash with deionized water and ethanol solution, filter to neutral, place in a vacuum oven, and vacuum dry at 80°C for 12 h to obtain a Si@C composite material.
将Si@C复合材料和氧化石墨烯按照质量比为10:1称取，加入到20mL水中，超声15min，使之充分分散在水溶液中。利用喷雾热裂解装置，将混合液喷雾到管式炉中，在700℃的H2/Ar混合载气的还原作用下，还原制得Si@C@G颗粒，通过静电场作用进行收集。The Si@C composite material and graphene oxide were weighed according to a mass ratio of 10:1, added to 20 mL of water, and ultrasonicated for 15 min to fully disperse them in the aqueous solution. Using a spray pyrolysis device, the mixed solution is sprayed into a tube furnace, and under the reducing action of H2/Ar mixed carrier gas at 700 °C, the Si@C@G particles are reduced to obtain Si@C@G particles, which are collected by electrostatic field.
图1是砂磨后的粒径分布图，选取了实施例4中砂磨5h后的颗粒进行粒径测试，结果表明，砂磨可以使微米级SiO2的平均粒径分布在200nm左右，具有较好的研磨效果。Fig. 1 is the particle size distribution diagram after sand milling, selected the particle after sand milling 5h in embodiment 4 to carry out particle size test, the result shows, sand milling can make the average particle diameter distribution of micron-order SiO2 at about 200nm, has Better grinding effect.
图2是不同NaCl添加量下镁热后的X射线衍射图，该图表明，NaCl的添加量会影响SiC的生成，NaCl加量的增加，有利于SiC的减少。Figure 2 is the X-ray diffraction pattern after magnesium heating with different NaCl additions, which shows that the addition of NaCl will affect the formation of SiC, and the increase of NaCl addition is beneficial to the reduction of SiC.
图3是Si@C喷雾干燥后的粒径放大图，可以看出，形成了蓬松的球形材料，因而有利于缓解材料的体积膨胀。Figure 3 is an enlarged view of the particle size of Si@C after spray drying. It can be seen that a fluffy spherical material is formed, which is conducive to alleviating the volume expansion of the material.
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