Method and device for preparing single-phase nano epsilon-Fe3N or gamma'-Fe4N powder

A technology of -fe3n and -fe4n, which is applied in the field of preparation of iron nitride materials, can solve problems such as the difficulty in preparing nano-iron nitride powder, and achieve the effects of ensuring quality stability, narrow particle size distribution, and avoiding pollution

Inactive Publication Date: 2010-12-22
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is difficult to prepare single-phase nano-iron nitride powder

Method used

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  • Method and device for preparing single-phase nano epsilon-Fe3N or gamma'-Fe4N powder
  • Method and device for preparing single-phase nano epsilon-Fe3N or gamma'-Fe4N powder
  • Method and device for preparing single-phase nano epsilon-Fe3N or gamma'-Fe4N powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Preparation of single-phase nanometer γ'-Fe 4 The method of N powder is as follows.

[0049] (1) vacuuming, forced gas circulation

[0050] After filling the water-cooled crucible with pure iron raw materials (block shape, purity ≥ 99.99%), close the exhaust valve, open the valve of the exhaust branch pipe, open the valve of the powder outlet channel, start the vacuum pump and the turbomolecular pump in turn, and pump the reactor Vacuum to 3.0×10 -4 Pa. Then open the reactor air inlet flowmeter to charge the protective gas (Ar gas), the inflation pressure is 0.05MPa, turn off the turbomolecular pump at the same time, turn off the vacuum pump after the inflation is completed, and turn on the variable frequency Roots pump to realize the protection gas passing through the reactor, Forced circulation and cooling of powder outlet channel, powder collection chamber, exhaust pipe, exhaust branch pipe, variable frequency Roots pump and condenser. The circulation velocity is...

Embodiment 2

[0058] Preparation of single-phase nanometer γ'-Fe 4 The method of N powder is as follows.

[0059] (1) vacuuming, forced gas circulation

[0060] After filling the water-cooled crucible with pure iron raw materials (block shape, purity ≥ 99.99%), close the exhaust valve, open the valve of the exhaust branch pipe, open the valve of the powder outlet channel, start the vacuum pump and the turbomolecular pump in turn, and pump the reactor Vacuum to 5.0×10 -4 Pa. Then open the reactor inlet flow meter to charge the reaction gas (N 2 ), the inflation pressure is 0.1MPa, and the turbomolecular pump is turned off at the same time. Forced circulation and cooling of gas branch pipe, variable frequency Roots pump and condenser, the circulation flow rate range is 5m / s. The circulating gas passes through the condenser, which is a shell and tube condenser, and the ice-water mixture with a temperature of 0°C is used as the cooling medium, and the gas can be cooled to 10°C.

[0061] (...

Embodiment 3

[0068] Preparation of single-phase nanometer γ'-Fe 4 The method of N powder is as follows.

[0069] (1) vacuuming, forced gas circulation

[0070] After filling the water-cooled crucible with pure iron raw materials (block shape, purity ≥ 99.99%), close the exhaust valve, open the valve of the exhaust branch pipe, open the valve of the powder outlet channel, start the vacuum pump and the turbomolecular pump in turn, and pump the reactor Vacuum to 1.0×10 -4 Pa. Then open the reactor inlet flow meter to charge the reaction gas (NH 3 ), the inflation pressure is 0.01MPa, and the turbomolecular pump is turned off at the same time. Forced circulation and cooling of gas branch pipe, variable frequency Roots pump and condenser, the circulation flow rate range is 1m / s. The circulating gas passes through the condenser, which is a shell and tube condenser, and the ice-water mixture with a temperature of 0°C is used as the cooling medium, and the gas can be cooled to 1°C.

[0071] ...

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Abstract

The invention relates to a method and a device for preparing single-phase nano epsilon-Fe3N or gamma'-Fe4N powder, and the device consists of a plasma evaporation powder making system, a powder collecting and modifying system, a vacuum system and a circulating system. The process steps for preparing the single-phase nano epsilon-Fe3N or gamma'-Fe4N powder are as follows: carrying out vacuum pumping and forced gas circulation, then carrying out plasma evaporation powder making, further carrying out powder modification, controlling the volume flow ratio of ammonia to hydrogen to be (1.4-1.6): 1, controlling the temperature in a powder trapping room at 345-355 DEG C, keeping the temperature for 5-7h, and obtaining the nano single-phase gamma'-Fe4N powder; and controlling the volume flow ratio of the ammonia to the hydrogen to be (2.4-2.6): 1, controlling the temperature in the powder trapping room at 445-455 DEG C, keeping the temperature for 1-3h and obtaining the nano single-phase epsilon-Fe3N powder. The method and the device can ensure that the product is the high-purity single-phase nano iron nitride powder through the precise control of reaction atmosphere.

Description

technical field [0001] The invention belongs to the technical field of magnetic materials, and in particular relates to a preparation method and device for iron nitride materials. Background technique [0002] Iron nitride mainly includes Fe 2 N, ε-Fe 3 N, γ'-Fe 4 N and α″-Fe 16 N 2 Most of them have excellent soft magnetic properties and good corrosion resistance and oxidation resistance, and are ideal magnetic recording media, magnetic induction elements and wave-absorbing materials. For example, γ′-Fe 4 The specific saturation magnetization of N phase is 193emu / g, slightly lower than that of pure iron (208.5emu / g). The density is 7.18g / cm 3 Lower than iron and iron-cobalt alloys. The Curie temperature is 767K, and it becomes metal-type conductive, and the chemical stability after passivation is far better than that of iron powder. In terms of magnetic properties, density, and oxidation resistance, γ'-Fe 4 N-phase is an excellent magnetic recording medium, magnet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06
Inventor 佟伟平王长久赫冀成
Owner NORTHEASTERN UNIV LIAONING
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