Molybdenum disulfide coated molybdenum dioxide anode material and preparation method and application thereof
A technology of molybdenum dioxide and molybdenum disulfide, which is applied to battery electrodes, electrical components, circuits, etc., can solve the problems of difficult sulfide etching, poor sulfide uniformity, and unsatisfactory electrical properties of materials, and achieve the effect of excellent specific capacity
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Embodiment 1
[0043] Calcination of MoO under an inert atmosphere 3 Obtain 0.03g / L molybdenum trioxide vapor, introduce it into the roasting chamber at 1150°C, and then blow in H at 0.01g / L 2 , mixed for 7 seconds, the gas-solid mixture was exported, and the solid product was cooled and separated to obtain molybdenum powder. The prepared metal molybdenum powder precursor was loaded into a quartz boat, placed in the heating zone of the tube furnace, and fed with a composition of 33% SO 2 , 67% Ar airflow, firstly heat up to 500°C at 20°C / min (first heating rate), then heat up to 700°C (calcination temperature) at 5°C / min (second heating rate), and heat at constant temperature for 60min, Stop heating, and take it out after cooling down to room temperature naturally with the furnace.
[0044] From figure 1 As shown in the XRD pattern, it can be seen that the prepared precursor is pure phase metal molybdenum; from figure 2 It can be seen from the TEM image shown that the synthesized metal ...
Embodiment 2
[0047] Using the same metal molybdenum precursor as in Example 1, the heating rate above 500°C was reduced to 2°C / min (the second heating rate), the calcination temperature was reduced to 650°C, and the calcination time was extended to 90min. As the heating rate slows down, the calcination temperature decreases, and the reaction rate also slows down accordingly. By prolonging the calcination time, the material can be synthesized slowly and uniformly.
[0048] Such as Figure 8 As shown, the molybdenum disulfide-wrapped molybdenum dioxide material prepared under this condition has at least one dimension of 30-60 nm. Compared with Example 1, not only the particle size is smaller, but the particle agglomeration phenomenon is also reduced. The molybdenum disulfide-wrapped molybdenum dioxide material was made into an electrode for electrochemical testing. After 130 cycles at a charge-discharge current of 200mA / g, it was found that the specific capacity of the negative electrode was...
Embodiment 3
[0050] Commercially available spherical metallic molybdenum powder with a size of 50 nm was used as a precursor, and the molybdenum disulfide-wrapped molybdenum dioxide material was prepared using the same synthesis conditions as in Example 1. Such as Figure 9 As shown, the particle size reached more than 100nm after calcination, and the agglomeration was serious. Electrodes made of this material are used for electrochemical tests, such as Figure 10 As shown, under the charge and discharge current of 200mA / g, after 130 cycles of circulation, the specific capacity of the negative electrode is maintained at about 700mAh / g, and the specific capacity can still reach about twice that of the commercially available graphite negative electrode. The performance of the anode material synthesized from the prepared metal molybdenum precursor is obviously declined.
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