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Iron nitride nano-powder and preparation method thereof

A technology of nano-powder and iron nitride, which is applied in the direction of chemical instruments and methods, nanotechnology, nitrogen compounds, etc., can solve the problems of complex process and low purity of iron nitride nano-powder, and achieve simple process and improved Agglomeration of product particles and the effect of preventing self-sintering

Active Publication Date: 2021-04-30
HEBEI LIFU CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a nano-iron nitride powder and its preparation method to solve the problems of low phase purity and complicated process of the iron nitride nano-powder prepared in the prior art

Method used

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  • Iron nitride nano-powder and preparation method thereof
  • Iron nitride nano-powder and preparation method thereof
  • Iron nitride nano-powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 50g of metal Fe powder with a purity of 99.99wt% and a particle size of 50nm in a glove box, and then weigh 10g of a reaction additive NH with a purity of 99.9%. 4 F powder (additive A), after fully mixing for 20 minutes, spread it in a molybdenum crucible. Put the mixed materials into the quartz sintering furnace, vacuumize to 20KPa, feed nitrogen-hydrogen mixed gas with a volume ratio of 1:1, control the flow rate at 1.5L / min, and then raise the temperature to 350°C at a rate of 5°C / min , then turn off N 2 , into NH 3 , H 2 and NH 3 The volume ratio is 1:3, and the temperature is raised to 550°C at a rate of 2°C / min, and kept for 3h, then turn off the NH 3 and H 2 , into N 2 The temperature was lowered to 200°C at a rate of 5°C / min, and then naturally cooled to room temperature to obtain a sintered product, which was pulverized and classified to obtain iron nitride below 100nm, which was characterized as follows: figure 1 and figure 2 shown.

[0024] R...

Embodiment 11-15

[0032] With reference to the preparation method of Example 1, the particle size of the raw iron powder was changed, and other process conditions were the same as in Example 1. The N content and particle morphology of the obtained iron nitride powder were tested, and the obtained results are shown in Table 2. shown.

[0033] Table 2

[0034]

[0035] It can be seen from Table 2 that the particle size of the raw material iron powder directly affects the particle size of the product, and the product particle size can be adjusted by changing the particle size of the raw material as required.

Embodiment 16-29

[0037] With reference to the preparation method of embodiment 1, change sintering temperature, H 2 and NH 3 The volume ratio and other process conditions are the same as in Example 1. The N content and particle morphology of the obtained iron nitride powder were tested, and the results are shown in Table 3.

[0038] table 3

[0039]

[0040]

[0041] It can be seen from Table 3 that by changing the sintering temperature and H 2 and NH 3It can be seen from the volume ratio that as the sintering temperature increases, the nitrogen content first increases and then decreases, and the particles agglomerate and the particle size becomes larger; when the sintering temperature is 550°C and the holding time is 3h, H 2 and NH 3 The volume ratio is 1:3, the particle uniformity is the best, the agglomeration is less, and the dispersion is good.

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Abstract

The invention provides iron nitride nano-powder and a preparation method thereof, the main phase of the powder is Fe4N, the nitrogen content is greater than or equal to 4.9 wt% and greater than or equal to 5.81 wt%, and the particle size of the powder is less than 100nm. The preparation method comprises the following steps: adding an additive NH4F into specific iron powder, controlling the reaction atmosphere, controlling the reaction process to sinter, and finally crushing and grading to obtain the product. The prepared iron nitride powder is high in pure phase degree, uniform in particle size, good in dispersity, simple in preparation method process, easy to operate and low in cost, the pure phase degree of the iron nitride powder is greatly improved, the particle size is controllable, the yield is high, the batch performance is stable, and industrial large-scale production can be conducted.

Description

technical field [0001] The invention relates to a nitride nanometer material, in particular to an iron nitride nanometer powder and a preparation method thereof. Background technique [0002] Iron nitride has good hardness and corrosion resistance. At the same time, iron nitride is also a good magnetic material, especially nanoscale iron nitride is an ideal raw material for preparing magnetic liquids and magnetic devices. Ferronitride ferrofluid is a new type of functional material developed in the past ten years. Because it has both magnetism and fluidity, it has advantages that general solid magnetic materials do not have. It is widely used in chemical industry, machinery, instrumentation, environmental protection and medical treatment, etc. has been widely applied. In the field of catalysis, iron nitride is an effective catalyst for many reactions (for example, for ammonia synthesis, Fischer-Tropsch synthesis, and electrocatalytic redox reactions), among which magnetic f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06B82Y40/00
CPCC01B21/0622B82Y40/00C01P2004/64C01P2004/03C01P2002/72
Inventor 杨志平许明亮郭静刘学千李璇璇赵金鑫蒋丽涛尤泳王大伟
Owner HEBEI LIFU CHEM TECH
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