Preparation method of nitrided iron nano-powder and high-pressure gas-solid reaction bed thereof

A high-pressure gas-solid reaction and nano-powder technology, which is applied in nanotechnology, nanotechnology, nitrogen-metal/silicon/boron binary compounds, etc., can solve the difficulty of airflow transporting nano-powders, small amount of plasma powder making, very high It is difficult to collect all of them, so as to achieve the effect of improving primary utilization rate, large batch output and improving reaction conditions

Inactive Publication Date: 2015-07-01
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main disadvantages of the above-mentioned disclosed method and device are: the amount of powder produced by plasma is small, it is difficult to transport the nano-powder by air flow and it is difficult to collect them all, the particle size of the nano-powder is small and it is easy to block the pipeline, and the reaction temperature under vacuum or normal pressure high wasted energy

Method used

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  • Preparation method of nitrided iron nano-powder and high-pressure gas-solid reaction bed thereof
  • Preparation method of nitrided iron nano-powder and high-pressure gas-solid reaction bed thereof
  • Preparation method of nitrided iron nano-powder and high-pressure gas-solid reaction bed thereof

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Effect test

Embodiment 1

[0027] Such as figure 1 , figure 2 As shown, the product particle size is Fe with an average particle size of 50±5nm 4 The preparation method of N nano powder and the high-pressure gas-solid reaction bed device, the specific operation steps are as follows:

[0028] 1. Weigh 1692 grams of FeCl 3 ·6H 2 O is put into a container, and is mixed with 8L water and 2L absolute ethanol to prepare stable precursor solution A; Get 751.47 grams of sodium hydroxide, dissolve in 10L twice distilled water and prepare stable precursor solution B; Precursor solution A and B are quickly mixed and reacted in the reactor to obtain a precipitated precursor, which is filtered, washed and dried with deionized water to obtain dark red iron hydroxide powder.

[0029] 2. Put the precursor ferric hydroxide powder through the opening of the quick connector 4 through the pipeline above the heater 3, put it into the high-pressure gas-solid reaction bed, first pass the gas inlet 9 into the nitrogen cle...

Embodiment 2

[0032] Such as figure 1 , figure 2 As shown, Fe with an average particle size of 80±5nm 4 The preparation method of N nano powder and its high-pressure gas-solid reaction bed, the specific operation steps are as follows:

[0033] Step one, step two are the same as embodiment 1.

[0034]Step 3, the temperature of the high-pressure gas-solid reaction bed is raised to 380°C through the heater 3, and the other procedures are the same as in Example 1 to finally obtain Fe 4 N nano-powder, the average particle size of the product is 80±5nm. Such as Figure 5 shown, for Fe 4 TEM picture of N nanopowder (380°C).

Embodiment 3

[0036] Such as figure 1 , figure 2 As shown, Fe 3 The preparation method of N nano powder and its high-pressure gas-solid reaction bed, the specific operation steps are as follows:

[0037] Step one, step two are the same as embodiment 1.

[0038] Step 3, use the exhaust valve of the circulation system to control and maintain the system pressure at 0.4-0.5MPa, and the other processes are the same as in Example 1 to finally obtain Fe 3 N nano powder. Such as Figure 6 Shown, for Fe 3 X-ray diffraction pattern of N nanopowder.

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Abstract

The invention discloses a preparation method of nitrided iron nano-powder and a high-pressure gas-solid reaction bed of the nitrided iron nano-powder and effectively prepares the nitrided iron nano-powder in an energy-saving mode. The preparation method of the nitrided iron nano-powder comprises the following steps: ferric salt and alkali precipitator are quickly mixed in a reactor, and ferric hydroxide powder is obtained after the reaction; the ferric hydroxide powder is put into the high-pressure gas-solid reaction bed, and ammonia and gas storage tank gas are ventilated to conduct the reaction; under a sealing condition, reaction resultant is discharged into a material storage tank, and finally the required the crystal type nitrided iron nano-powder is obtained. The high-pressure gas-solid reaction bed of the nitrided iron nano-powder comprises a gas sparger, a powder supporting net, a heater, a quick connector, a material storage tank valve, a material storage tank, a heating power source, a thermocouple, a gas inlet valve, a gas inlet, a gas outlet valve, a gas outlet, a reaction bed side wall and a ventilation valve. The preparation method of the nitrided iron nano-powder and the high-pressure gas-solid reaction bed of the nitrided iron nano-powder are simple in operation and energy-saving, the rection equipment can be connected in parallel, and the batch production amount is big.

Description

technical field [0001] The invention relates to a method for preparing metal nitride nano powder and a device thereof, in particular to a method for preparing iron nitride nano powder and a high-pressure gas-solid reaction bed thereof. Background technique [0002] Solid-state nitrides have attracted attention due to their properties for engineering applications. For example, some transition metal nitrides have high strength, high hardness, and good thermal and electrical conductivity. Iron nitride has good hardness and corrosion resistance, and is widely used in the fields of machining and metal surface treatment. Iron nitride is a good magnetic material, and nanoscale iron nitride is used to prepare magnetic liquids and magnetic materials. It is an ideal raw material for devices. In the field of catalysis, iron nitride is an effective catalyst for many reactions. For example, the catalysis of ammonia synthesis, Fischer-Tropsch synthesis and hydrazine decomposition reactio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/06B82Y30/00
Inventor 李晓奇王开明高首山
Owner UNIV OF SCI & TECH LIAONING
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