Research on preparation of nano sodium vanadium phosphate and its sodium storage properties
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摘要: 基于磷酸钒钠制备条件苛刻、颗粒粒径大、电导率差等问题，提出了一种制备纳米磷酸钒钠的新方法。通过碱性沉钒形成羟基氧化钒，再利用PO43-、F-等阴离子与OH-的原位离子交换，从而得到纳米化的磷酸钒钠。借助XRD、SEM、FTIR等方法，分析了纳米磷酸钒钠的形成机理，优化了合成条件。电化学测试结果表明，磷酸钒钠的纳米化提升了电子/离子输运能力，使得所制备的纳米磷酸钒钠表现出优异的储钠性能。当电流密度为10 mA/g时，其放电比容量为106.68 mAh/g，并且循环20次循环充放电后，仍能保持80.85 mAh/g的放电比容量。Abstract: Based on the severe preparation conditions, large particle size and poor conductivity, a new method to prepare sodium vanadium phosphate was proposed. By the formation of alkaline vanadium compounds, vanadium hydroxyloxide, and the in-situ anions exchange reactions between PO43–, F– and OH–, nano vanadium sodium phosphate was consequently obtained. With the help of XRD, SEM, FTIR, the formation mechanism of nano vanadium sodium phosphate was analyzed, and the synthesis conditions were optimized. The electrochemical test results show that the sodium vanadium phosphate in nanoscale improves the electron/ion transport capacity, and makes the prepared sodium vanadium phosphate show excellent sodium storage performances. When the current density is 10 mA/g, the specific discharge capacity is 106.68 mAh/g. At the same time, the specific discharge capacity of 80.85 mAh/g can be maintained after 20 charge and discharge cycles.
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图 1 纳米磷酸钒钠制备流程示意
Figure 1. Schematic diagram of the preparation of nano sodium vanadium phosphate
图 2 羟基氧化钒与纳米磷酸钒钠的物相信息表征
Figure 2. Characterization of hydroxy vanadium oxide and sodium vanadium phosphate
图 3 沉钒率与NaOH添加量的关系
Figure 3. Relationship between vanadium precipitation rate and NaOH amounts
图 4 不同热处理温度下磷酸钒钠的XRD谱
Figure 4. XRD of sodium vanadium phosphate at different post-treatment temperatures
图 5 不同热处理温度下磷酸钒钠的红外光谱
Figure 5. FTIR of sodium vanadium phosphate at different post-treatment temperatures
图 6 不同后处理温度下的磷酸钒钠样品的SEM形貌
Figure 6. SEM of sodium vanadium phosphate samples at different post-treatment temperatures
图 7 不同后处理温度下的磷酸钒钠样品的激光粒度分布表征
Figure 7. Characterization of the particle size distribution of sodium vanadium phosphate samples at different post-treatment temperatures
图 8 纳米磷酸钒钠扣式半电池的储钠性能表征
Figure 8. Characterization of sodium-storage performances of the obtained sodium vanadium phosphate sodium ions battery
表 1 不同NaOH添加量下，羟基氧化钒的产量变化情况
Table 1. Changes in the yield of hydroxy vanadium oxide under different NaOH additions
VOSO4/
mLNaOH
添加量/gNaOH
浓度/(mol·L−1)混合
pH羟基氧化
钒产量/g沉钒
率/%10 0.1 0.25 3.36 0.0851 8.42 10 0.2 0.5 3.48 0.3245 32.13 10 0.3 0.75 3.62 0.4720 46.73 10 0.4 1 3.78 0.5514 54.59 10 0.5 1.25 3.85 0.7831 77.83 10 0.6 1.5 5.54 0.822 81.39 10 0.7 1.75 9.52 0.4534 44.89 10 0.8 2.0 12.53 0.2404 23.80 
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