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采用热丝化学气相沉积法制备B掺杂纳米金刚石薄膜,并对薄膜进行真空退火处理,系统研究了不同退火温度对B掺杂纳米金刚石薄膜的微结构和电化学性能的影响.结果表明,当退火温度升高到800℃后,薄膜的Raman谱图中由未退火时在1157,1346,1470,1555cm-1处的4个峰转变为只有D峰和G峰,说明晶界上的氢大量解吸附量减少;并且D峰和G峰的积分强度比ID/IG值变为最小,即sp2相团簇数量减少或尺寸变小;G峰左移,石墨相无序化程度增加;此时电极具有最宽的电势窗口和最高的析氧电位,电极表面进行可逆电化学反应.1000℃退火时,D峰增强,峰较尖锐,ID/IG值最大,并且石墨相有序化程度增加,电极具有最窄的电势窗口和最低的析氧电位,电极表面进行可逆电化学反应.不同退火温度下,纳米金刚石薄膜中sp2相团簇数量或尺寸、晶界上聚集的与氢有关的反式聚乙炔的量、石墨相的无序化程度以及B的扩散使得薄膜的电化学性能随退火温度的升高呈复杂的变化。
The effects of annealing temperature on the microstructure and electrochemical performance of B-doped nano-diamond films were investigated systematically by hot wire chemical vapor deposition (CVD) method. The results show that when After the annealing temperature was raised to 800 ℃, the Raman spectra of the films were changed from four peaks at 1157, 1346, 1470 and 1555 cm-1 to only D-peak and G-peak at the time of un-annealed, indicating that a large amount of hydrogen The desorption amount decreased; and the integral intensities of D peak and G peak became smaller than that of ID / IG, that is, the number of clusters in sp2 phase decreased or decreased in size; the shift of G peak left and the degree of disorder of graphite phase increased; The electrode has the widest potential window and the highest oxygen evolution potential, and the electrode surface undergoes a reversible electrochemical reaction.When annealing at 1000 ℃, the D peak is enhanced, the peak is sharper, the ID / IG value is the largest, and the order of the graphite phase is increased, Electrode has the narrowest potential window and the lowest oxygen evolution potential, the electrode surface reversible electrochemical reactions.At the different annealing temperature, the number or size of sp2 phase clusters in nanodiamond films, the hydrogen-dependent trans The amount of polyacetylene, graphite phase disorder process B and the diffusion of the electrochemical properties of the film such that the annealing temperature was elevated with complex changes.