A kind of preparation method of tungsten nitride nano rod
A tungsten nitride nanometer and tungstate technology, applied in chemical instruments and methods, nitrogen compounds, nanotechnology and other directions, can solve the problems of long preparation time and low synthesis efficiency, and achieve low cost, low equipment requirements and simple process. Effect
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Embodiment 1
[0026] Weigh 25g of sodium tungstate and 10g of oxalic acid and put them into a ball mill jar, mill them in a planetary ball mill for 2 hours, take out the milled materials and balls, dry them in a blast oven at 60°C for 2 hours, and put the dried product in water Wash, filter, and dry to obtain the tungsten trioxide precursor, carry out XRD analysis on the tungsten trioxide precursor, the results are as follows figure 1 Shown, XRD patterns and WO 3 The JCPDS No. 85-2460 coincides with the SEM analysis of the tungsten trioxide precursor, and the results are as follows figure 2 As shown, WO 3 It is nanosheets, uniformly dispersed; then the precursor is placed in a calciner, and a mixed gas with a volume ratio of hydrogen and nitrogen of 1:17 is introduced at a flow rate of 15ml / min, and the temperature is increased from room temperature at a rate of 10°C / min. Raise it to 800°C, keep it warm for 2 hours, and after cooling, tungsten nitride nanorods are obtained. Carry out XR...
Embodiment 2
[0028] Weigh 25g of sodium tungstate and 21g of citric acid and put them into a ball mill jar, mill them in a planetary ball mill for 3 hours, take out the milled materials and balls, dry them in a blast oven at 60°C for 2 hours, and put the dried product Wash with water, filter, and dry to obtain a tungsten trioxide precursor, then place the precursor in a calcination furnace, and feed a mixed gas with a volume ratio of hydrogen and nitrogen of 1:17 at a flow rate of 20ml / min, at 10°C / min The heating rate is increased from room temperature to 750° C., and after cooling for 3 hours, tungsten nitride nanorods are obtained. SEM analysis of tungsten nitride nanorods, the results are as follows Figure 5 As shown, WN is a cluster of nanorods.
Embodiment 3
[0030] Weigh 25g of sodium tungstate and 17g of tartaric acid and put them into a ball mill jar, mill them in a planetary ball mill for 2 hours, take out the milled materials and balls, dry them in a blast drying oven at 60°C for 2 hours, and put the dried products in water Wash, filter, and dry to obtain a tungsten trioxide precursor, then place the precursor in a calciner, and feed a mixed gas with a volume ratio of hydrogen and nitrogen of 1:17 at a flow rate of 15ml / min, and at a rate of 10°C / min The heating rate is raised from room temperature to 800° C., and the temperature is kept for 2 hours. After cooling, tungsten nitride nanorods are obtained.
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