Black phosphorus preparation method with high conversion rate
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A high-conversion, black phosphorus technology, applied in the preparation of phosphorus, electrical components, battery electrodes, etc., can solve the problems of low yield, ultra-high pressure, high toxicity, etc., and achieve simple steps, high conversion rate, and good crystallinity Effect
Inactive Publication Date: 2015-01-28
ZHEJIANG UNIV
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However, because the above-mentioned methods for synthesizing black phosphorus often have high toxicity, low yield, and need ultra-high pressure, high temperature and other deficiencies, it is urgent to improve the preparation process of black phosphorus
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Embodiment 1
[0014] Mix red phosphorus, tin and tin tetraiodide in a mass ratio of 3:40:1, put them into a quartz tube, evacuate until the pressure inside the quartz tube is less than 0.05pa, seal the tube, and heat to make the temperature of the raw material end in the quartz tube The temperature was 200°C, then raised to 600°C in 1 hour, kept at 6 hours, then cooled to 300°C in 6 hours, kept at 2 days, cooled to room temperature in 10 hours, and the product was taken out.
[0015] The product obtained was a black mass, figure 1 Its XRD figure, its SEM such as figure 2 As shown, it can be seen that the obtained product is black phosphorus. And after measurement, the mass of black phosphorus obtained is about 97% of the mass of red phosphorus in the raw material.
Embodiment 2
[0017] Mix red phosphorus, tin and tin tetraiodide in a mass ratio of 3: 25: 1, put them into a quartz tube, evacuate until the pressure inside the quartz tube is less than 0.05pa, seal the tube, and heat to make the temperature of the raw material end in the quartz tube It takes 2 hours to raise the temperature to 700°C, keep it warm for 10 hours, then take 8 hours to cool it down to 500°C, keep it for 3 days, then take 15 hours to cool down to room temperature, and black phosphorus is obtained in the quartz tube.
Embodiment 3
[0019] Mix red phosphorus, tin and tin tetraiodide in a mass ratio of 1:40:1, put them into a quartz tube, evacuate until the pressure inside the quartz tube is less than 0.05pa, seal the tube, and heat to make the temperature of the raw material end in the quartz tube The temperature is 100°C, then raised to 400°C in 1 hour, kept at 5 hours, then lowered to 200°C in 6 hours, kept at 1 day, lowered to room temperature in 10 hours, and black phosphorus was obtained in the quartz tube.
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Abstract
The invention discloses a black phosphorus preparation method with a high conversion rate. The preparation method comprises the following steps: mixing red phosphorus, tin and tin tetraiodide in a mass ratio of (1-6):(40-50):(1-2), filling the mixture into a quartz tube, vacuumizing until the pressure in the quartz tube is smaller than 0.05 Pa, sealing the tube, heating to ensure that the raw material end temperature in the quartz tube is 100-400 DEG C, heating to 400-700 DEG C in 1-2 hours, keeping the temperature for 5-10 hours, then cooling to 200-500 DEG C in 6-8 hours, keeping the temperature for 1-3 days, and finally cooling to the room temperature in 10-15 hours to obtain black phosphorus. The preparation method disclosed by the invention is simple in step and strong in operability; on the one hand, a nontoxic raw material is adopted to achieve effects of cleanliness and environmental friendliness, and on the other hand, only a mild reaction condition is needed, so that the energy consumption and cost are reduced, and the prepared black phosphorus has good crystallinity and a high conversion rate. The preparation method disclosed by the invention has strong repeatability and is favorable for industrial popularization and application.
Description
technical field [0001] The invention relates to a method for preparing black phosphorus, in particular to a method for preparing black phosphorus with a high conversion rate, and belongs to the field of synthesis of chemical materials. technical background [0002] The development and application of new materials is one of the main directions of scientific development in this century. In 2004, the successful preparation of graphene caused great waves in the scientific community. Due to its high conductivity, high toughness and large specific surface area, it is considered to be expected to replace the traditional semiconductor silicon, triggering a new wave in the field of electronic technology. round of research boom. However, since graphene has no energy band, it cannot realize the on and off of logic circuits, which greatly limits its application in the fields of electronic devices and optoelectronic devices, such as field effect transistors, photodetectors, solar cells,...
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