New method for preparing ternary molybdenum nitride nano material

A nanomaterial and nitride technology, applied in the field of nanomaterials, can solve the problems of low purity of ternary molybdenum nitrides, and achieve the effects of simple and easy-to-control reaction process, wide source of raw materials and low reaction temperature.

Active Publication Date: 2017-12-29
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These prepared ternary molybdenum nitrides have relatively low purity, and toxic ammonia gas is utilized as nitrogen source (J.Alloy.Compd.291(1999) 94.)

Method used

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  • New method for preparing ternary molybdenum nitride nano material
  • New method for preparing ternary molybdenum nitride nano material
  • New method for preparing ternary molybdenum nitride nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]Add 5mmol of metallic molybdenum powder, 10mmol of ferric oxide and 80mmol of sodium azide to a 20ml stainless steel autoclave, seal it and put it into an electric furnace capable of temperature programming, and the furnace temperature rises from room temperature to 80 minutes. 800°C, then maintained at 800°C for 5 hours and then naturally cooled to room temperature. The final product in the autoclave included black deposits and residual gas. Collect the black deposits that stick to the inner surface of the kettle wall, wash them with distilled water and absolute ethanol for many times, and filter the obtained samples. The samples were dried in a vacuum drying oven at 50 °C for 4 hours, and finally collected for characterization. .

[0037] The phase analysis of the powder was carried out using a Japanese Rigaku D / max-γA X-ray powder diffraction (XRD) instrument. Graphite monochromator, the tube voltage and current are 40kV and 20mA, respectively, and the scanning spe...

Embodiment 2

[0039] 5mmol metal molybdenum powder, 10mmol cobalt chloride and 80mmol sodium azide were added to a 20ml stainless steel autoclave, sealed and put into an electric furnace capable of temperature programming, and the furnace temperature was raised from room temperature to 800 ℃ within 80 minutes. °C, and then maintained at 800 °C for 5 hours and then naturally cooled to room temperature. The final product in the autoclave included black deposits and residual gas. Collect the black deposits that stick to the inner surface of the kettle wall, wash them with distilled water and absolute ethanol for many times, and filter the obtained samples. The samples were dried in a vacuum drying oven at 50 °C for 4 hours, and finally collected for characterization. .

[0040] Figure 5 The X-ray diffraction pattern of the product prepared in Example 2. Depend on Figure 5 It can be seen that in the X-ray diffraction spectrum, 2θ has all diffraction peaks at 10-80°, in which the diffracti...

Embodiment 3

[0042] 5mmol metal molybdenum powder, 10mmol nickel chloride and 80mmol sodium azide were added to a 20ml stainless steel autoclave, sealed and put into an electric furnace capable of temperature programming, and the furnace temperature was raised from room temperature to 800 ℃ within 80 minutes. °C, and then maintained at 800 °C for 5 hours and then naturally cooled to room temperature. The final product in the autoclave included black deposits and residual gas. Collect the black deposits that stick to the inner surface of the kettle wall, wash them with distilled water and absolute ethanol for many times, and filter the obtained samples. The samples were dried in a vacuum drying oven at 50 °C for 4 hours, and finally collected for characterization. .

[0043] Figure 10 For the X-ray diffraction pattern of the product prepared in Example 3, all diffraction peaks in the figure can be designated as cubic phase ternary nitrides No other impurity peaks appeared. The morphol...

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Abstract

The invention relates to a synthesis method of a ternary molybdenum nitride. The synthesis method is characterized in that a ternary molybdenum nitride (TnMo3N) nano material is prepared under a mild condition by adopting one-step chemical reaction; the synthesis method comprises the following steps: accommodating metal molybdenum powder, a metal T source compound and sodium azide in a reaction kettle, and heating to 600 to 800 DEG C, wherein the reaction time is 5 to 40 hours; cooling; washing a product; filtering, separating and drying, thus obtaining the ternary molybdenum nitride (TnMo3N) nano material, wherein the yield is up to 90 percent or more.

Description

technical field [0001] The invention belongs to the field of nanomaterials, in particular to a method for preparing ternary molybdenum-based nitride nanomaterials under mild conditions. Background technique [0002] Transition metal nitrides are a class of "filled" compounds formed by nitrogen atoms entering the metal lattice. These materials have electronic properties similar to those of the noble metal Pt, and perform well in ammonia synthesis and decomposition and organic synthesis reactions. catalytic performance. Ternary molybdenum nitride (Fe 3 Mo 3 N, Co 3 Mo 3 N and Ni 2 Mo 3 N) possesses both excellent catalytic and magnetic properties. [0003] At present, the preparation of ternary molybdenum nitride (Fe 3 Mo 3 N, Co 3 Mo 3 N and Ni 2 Mo 3 The method of N) is mainly through two-step synthesis, the first step is to prepare the corresponding ternary oxide (FeMoO 4 , CoMoO 4 and NiMoO 4 ), and in the second step, a ternary molybdenum-based nitride is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06B82Y40/00
CPCC01B21/0602C01P2002/72C01P2002/88C01P2004/03C01P2004/04C01P2004/38C01P2004/62C01P2004/64C01P2006/42
Inventor 王良彪秦恒飞张开龙刘维桥周全法钱逸泰
Owner JIANGSU UNIV OF TECH
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