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A method for preparing ternary molybdenum-based nitride nanomaterials

A nanomaterial and nitride technology, which is 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 price.

Active Publication Date: 2020-02-14
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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  • A method for preparing ternary molybdenum-based nitride nanomaterials
  • A method for preparing ternary molybdenum-based nitride nanomaterials
  • A method for preparing ternary molybdenum-based nitride nanomaterials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]Add 5mmol metal molybdenum powder, 10mmol ferric oxide and 80mmol sodium azide into 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 800°C, then maintained at 800°C for 5 hours and then cooled to room temperature naturally. The final product in the autoclave consisted of black deposits and residual gas. Collect the black sediment stuck on the inner surface of the kettle wall, wash it with distilled water and absolute ethanol several times, filter the sample obtained, and dry the sample in a vacuum drying oven at 50°C for 4 hours, and finally collect it for characterization .

[0037] The phase analysis of the powder was carried out by a Japanese Rigaku D / max-γA X-ray powder diffraction (XRD) instrument, Cu Kα Graphite monochromator, tube voltage and current are 40kV and 20mA, scanning speed 10.0° min -1 . figure 1 It is the X-ray diffraction sp...

Embodiment 2

[0039] Add 5mmol metal molybdenum powder, 10mmol cobalt chloride and 80mmol sodium azide into 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 800 within 80 minutes °C, and then maintained at 800 °C for 5 hours and then cooled to room temperature naturally. The final product in the autoclave consisted of black deposits and residual gas. Collect the black sediment stuck on the inner surface of the kettle wall, wash it with distilled water and absolute ethanol several times, filter the sample obtained, and dry the sample in a vacuum drying oven at 50°C for 4 hours, and finally collect it for characterization .

[0040] Figure 5 It is the X-ray diffraction spectrogram 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 10-80o, among which the diffraction intensi...

Embodiment 3

[0042] Add 5mmol metal molybdenum powder, 10mmol nickel chloride and 80mmol sodium azide into 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 800 within 80 minutes °C, and then maintained at 800 °C for 5 hours and then cooled to room temperature naturally. The final product in the autoclave consisted of black deposits and residual gas. Collect the black sediment stuck on the inner surface of the kettle wall, wash it with distilled water and absolute ethanol several times, and filter the sample obtained, and dry the sample in a vacuum drying oven at 50°C for 4 hours, and finally collect it for characterization .

[0043] Figure 10 For the X-ray diffraction spectrum of the product prepared in embodiment 3, all diffraction peaks in the figure can be marked as the ternary nitride Ni of cubic phase 2 Mo 3 N No other impurity peaks appeared. The morpho...

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Abstract

The present invention relates to a kind of synthetic method of ternary molybdenum series nitride, this method adopts one-step chemical reaction to prepare ternary molybdenum series nitride (T n Mo 3 N) nanomaterials, metal molybdenum powder, metal T source compound, and sodium azide are placed in a reaction kettle, heated to 600-800 ° C, the reaction time is 5-40 hours, cooled, the product is washed, filtered and separated and dried , That is, the yield reaches more than 90%.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(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