How to Prepare Inorganic Fullerene Tungsten Disulfide nanotube? (I)

Inorganic fullerene tungsten disulfide nanotube has structure of concentric tube layers and can be widely used in many important fields. How to prepare inorganic fullerene WS₂ nanotube? The methods of thermal decomposition and direct heating can be taken, which are simple and time-saving.

Inorganic Fullerene (IF) tungsten disulfide nanotube has structure of concentric tube layers, which is the same as that of C60 and carbon nanotube. This special structure determines the excellent mechanical, friction and electronic transportation properties of inorganic fullerene tungsten disulfide nanotube, making it a useful and important material.

The two methods of preparing inorganic fullerene tungsten disulfide nanotube are as follow:

1. Thermal Decomposition

Step One：(NH4) ₂WS₄ is prepared by mixing (NH4) ₆W₁₂O₃₉ and NH₄S, and then (NH4) ₂WS₄ is crushed to amorphous or nanometer size by ball mill in H₂. And its surface area and reactivity are increased.

Step Two: The crushed (NH4) ₂WS₄ powder is placed and dispersed in a quartz crucible. The crucible is heated in a tubular furnace in the mixed atmosphere of H₂ and C₄H₄S. When the temperature up to 360°C, the crucible is kept warm for 30 minutes. And then it is cooled to room temperature under this atmosphere before inorganic fullerene tungsten disulfide nanotube is successfully prepared. C₄H₄S is used as catalyst in the reaction and the involved chemical formula is as follows:

(NH4) ₂WS₄+ H₂→WS₂+2H₂S-+2NH₃

2. Direct Heating

Step One：A stainless steel container with two stainless steel electrodes is used as the heating device in the preparation process. And the electrodes are cooled by water. The tungsten foil is connected with the electrodes and is located at the bottom of the container. The SiO₂ sheet is placed on the top of the stainless steel container.

Step Two: The whole container is filled with argon. And then the tungsten foil is given the current of 35 A for 30 minutes. Measured by optical thermometer, the temperature of the tungsten foil can reach 1200°C and it can be kept warm for 30 minutes.

Step Three: When WO_3-x (x=0~1) nanorods with a diameter of 10-100 nm and a length of 90 nm occur on the edge of SiO₂ sheet, H₂S is quickly injected into the stainless steel container. At the same time, the heating current is reduced to 30 A, and the temperature in the container is set at 1000°C. The container is kept warm for 30 min until the tree-like structure on the edge of SiO₂ sheet is turned into grey needle-like structure.

Step Four: The power is turned off. And when the container is cooled to room temperature, the product with needle-like structure is collected. Inorganic fullerene tungsten disulfide nanotube with complete structure and high purity is successfully prepared.

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