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Preparation method of high-yield high-purity MoO2 powder

A high-purity, high-yield technology, used in molybdenum oxide/molybdenum hydroxide and other directions, can solve the problems of limited large-scale preparation and production, strict control requirements, complex chemical reactions, etc., to achieve easy storage and reprocessing, and easy process. Controlled, high-purity effects

Inactive Publication Date: 2016-08-17
CHINA UNIV OF GEOSCIENCES (BEIJING)
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Problems solved by technology

The liquid-phase method consumes less energy than the gas-phase method, but the reaction time is long, the chemical reaction is complex, difficult to control, and requires subsequent purification and impurity removal processes. Therefore, the control requirements for reaction conditions are relatively strict, which limits its large-scale preparation and Production

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  • Preparation method of high-yield high-purity MoO2 powder
  • Preparation method of high-yield high-purity MoO2 powder

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preparation example Construction

[0026] High-yield, high-purity MoO proposed by the present invention 2 The preparation method of powder comprises the following steps and content:

[0027] (1) The evaporation source used is commercially available analytically pure MoO 3 powder and S powder. Among them, the evaporation source MoO 3 The grain size of the powder is between 2 and 5 μm, the evaporation source S powder is high-purity sulfur or sublimed sulfur, and the raw material MoO 3 The mass ratio of powder and S powder is controlled between 1:1 and 1:5.

[0028] (2) In the horizontal vacuum tube furnace, vertical vacuum box furnace, vertical vacuum tube furnace or well type vacuum electric furnace, the evaporation source MoO 3 Alumina ceramic crucibles of powder and S powder are placed in the heating area in the center of the furnace. Among them, the alumina ceramic crucible filled with S powder is placed above the air flow, and the MoO 3 The powdered ceramic crucible is placed under the airflow, and the...

Embodiment 1

[0033] Embodiment 1: In the horizontal vacuum tube furnace, the alumina ceramic crucible with 1g high-purity S powder and 0.5g analytically pure MoO are housed 3 The powdered alumina ceramic crucibles are respectively placed in the central heating zone of the furnace, and the distance between the two is 5cm.

[0034] Before heating, evacuate the whole system to 10 with a vacuum pump -2 Below Pa, then feed 99.99vol.% argon into the system, and repeat 3 times to get rid of the residual air in the system. Then the temperature was raised to 950°C at a rate of 30°C / min, and kept for 1 hour. During the whole heating process, keep the carrier gas flow rate at 200 sccm under the premise of continuous operation of the vacuum pump, until the temperature is naturally cooled to room temperature, then the MoO 3 High-purity MoO was obtained in a crucible of powder 2 Powder.

[0035] The obtained sample is crystalline MoO 2 , no impurity (see figure 1 ), showing obvious granular shape ...

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Abstract

The invention relates to a preparation method of high-yield high-purity MoO2 powder, belonging to the technical field of material preparation. In a vacuum heating furnace, molybdenum trioxide and sulfur powder used as raw materials are subjected to non-mixing prograde reaction by a heat evaporation vapor transport technique to reduce and synthesize the high-yield high-purity MoO2 powder by one step. The method has the advantages of strict and controllable synthesis conditions, simple equipment and technique, high product yield, low cost, high safety, environment friendliness and the like. The obtained MoO2 powder has the advantages of uniform particle size and high purity, and can be easily stored and reprocessed. The MoO2 powder has wide application prospects in the aspects of metallurgy, catalysts, lithium ion batteries and the like.

Description

technical field [0001] The invention relates to a high-yield and high-purity MoO 2 The preparation method of powder belongs to the technical field of material preparation. Background technique [0002] In addition to being a metallurgical additive, molybdenum dioxide (MoO 2 ) also has excellent optical and electrical properties, and is expected to be used in the manufacture of light-emitting diodes (OLEDs), liquid crystal displays (LCDs), ion display panels (PDPs), field emission display panels (FEDs) and other equipment. In particular, since MoO 2 The symmetry of the monoclinic structure in the structure is relatively low (Magneli A, Gerog, Andersson.On the MoO 2 Structure Type. Acta Chemica Scandinavica, 1955, 9:1378-1381), and MoO 2 The Mo atoms in each octahedron of the crystal are off-centre, making MoO 2 has metallic conductivity, so MoO 2 It can be used to make electrical devices, especially when it is used as an electrode material in a lithium-ion battery, it i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/02
CPCC01G39/02C01P2002/72C01P2004/03C01P2004/61C01P2006/80
Inventor 李汉青彭志坚钱静雯申振广符秀丽
Owner CHINA UNIV OF GEOSCIENCES (BEIJING)
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