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

A powder, single-phase technology, applied in the field of preparation of iron nitride materials, can solve the problem of difficulty in preparing nano-iron nitride powder, etc., and achieve the effects of ensuring quality stability, good powder dispersion and avoiding pollution

Inactive Publication Date: 2010-01-20
NORTHEASTERN UNIV
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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 for preparing single phase nanometer epsilon-Fe3N or gamma'-Fe4N powder and device thereof
  • Method for preparing single phase nanometer epsilon-Fe3N or gamma'-Fe4N powder and device thereof
  • Method for preparing single phase nanometer epsilon-Fe3N or gamma'-Fe4N powder and device thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Preparation of single-phase nanometer γ'-Fe 4 The method of N powder is as follows.

[0046] (1) vacuuming, forced gas circulation

[0047] 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

[0054] Preparation of single-phase nanometer γ'-Fe 4 The method of N powder is as follows.

[0055] (1) vacuuming, forced gas circulation

[0056] 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.

[0057] (...

Embodiment 3

[0063] Preparation of single-phase nanometer γ'-Fe 4 The method of N powder is as follows.

[0064] (1) vacuuming, forced gas circulation

[0065] 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.

[0066] (2...

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Abstract

The invention relates to a method for preparing single phase nanometer epsilon-Fe3N powder or gamma'-Fe4N powder and a device thereof; the device comprises a plasma evaporation pulverizing system, a powder collection and modification system, a vacuum system and a circulating system. The process for preparing single phase nanometer epsilon-Fe3N or gamma'-Fe4N powder comprises the following steps: vacuumizing, cycling gas compulsively, then performing plasma evaporation to prepare powder, then modifying the powder while ensurng that the cubic content ratio of ammonia to hydrogen is (1.4-1.6):1, the temperature of a powder catcher room is 345-355 DEG C and the temperature is kept for 5-7h and obtaining the single phase nanometer gamma'-Fe4N powder; or modifying the powder while ensurng that the cubic content ratio of ammonia to hydrogen is (2.4-2.6):1, the temperature of a powder catcher room is 445-455 DEG C and the temperature is kept for 1-3h and obtaining the single phase nanometer epsilon-Fe3N powder. By controlling the reaction atmosphere precisely, the product is ensured to be high purity single phase nanometer iron nitride powder.

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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IPC IPC(8): C01B21/06
Inventor 佟伟平王长久赫冀成
Owner NORTHEASTERN UNIV
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