Ultra-fine rare earth iron series magnetic alloy powder coprecipitation reduction scattering preparation

A magnetic alloy and co-precipitation technology, which is applied in the field of permanent magnet material preparation, can solve the problems that the particle size cannot reach the range of single-domain particle size, the magnetic performance of magnetic materials decreases, and the particle size of raw materials is large, so as to achieve complete grain structure and excellent magnetic properties. energy and reduce production costs

Inactive Publication Date: 2008-09-10
CENT SOUTH UNIV
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The particle size of the raw materials used in the current reduction diffusion method is still relatively large, not only will the alloy be severely oxidized due to the powerful ball milling, but also the particle size cannot reach the particle size range of the single domain region, and the magnetic properties of the subsequent magnetic materials will inevitably decline

Method used

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  • Ultra-fine rare earth iron series magnetic alloy powder coprecipitation reduction scattering preparation
  • Ultra-fine rare earth iron series magnetic alloy powder coprecipitation reduction scattering preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 1.7mol / L FeCl 2 solution and 0.2mol / L SmCl 3 Each solution was 100ml, mixed at room temperature, heated to 28°C to adjust pH=1.5; then take 1.0mol / L (NH 4 ) 2 C 2 o 4 200ml of solution, heated to 28°C to adjust pH=4.2; fast feed in parallel flow, feed speed control is based on pH=2.5. After the feeding was completed, the temperature was raised to 40° C., and aged for 1.0 h. The aging process is NH 3 ·H 2 O and HCl were used to adjust the pH value to 2.5, and the stirring speed was controlled to be 200 rpm during the feeding and aging process. After the aging is completed, filter and wash the precipitate with hot water until the anion cannot be detected; after drying, the samarium iron oxalate precursor powder Sm 2 (C 2 o 4 ) 3 10H 2 O and FeC 2 o 4 2H 2 O, with a weight of 38.2g. After testing, the molar ratio of iron and samarium is 8.5:1; X-ray diffraction results show that it is a good crystal form, the powder particle size is between 1 and 20 μm,...

Embodiment 2

[0022] Take 0.17mol / L FeCl 2 solution and 0.02mol / L SmCl 3 Each solution was 100ml, mixed at room temperature, heated to 32°C, and adjusted to pH=2.0; then take 0.1mol / L H 2 C 2 o 4 200ml of the solution was heated to 32°C, and the pH was adjusted to 2.4; the feed was fed rapidly in parallel, and the feeding speed was controlled so that the pH of the reaction mixture was 2.0. After the feeding is completed, raise the temperature to 50°C, and age for 1.0h. During the aging process, use NH 3 ·H 2 O and HCl were used to adjust the pH to 2.0, and the stirring speed was controlled at 200 rpm during the feeding and aging process. After aging, filter and wash the powder with hot water until the anions cannot be detected. After drying, 3.85g of samarium iron oxalate precursor powder Sm 2 (C 2 o 4 ) 3 10H 2 O and FeC 2 o 4 2H 2 O.

[0023] The obtained samarium iron oxalate precursor powder was in N 2 Atmosphere, temperature 760°C, time 4 hours for calcination treatment...

Embodiment 3

[0025] Take 1.7mol / L FeCl 2 solution and 0.2mol / L LaCl 3 Each solution was 100ml, mixed at room temperature, heated to 30°C, and adjusted to pH=2.0; then take 1.0mol / L (NH 4 ) 2 C 2 o 4 200ml of solution, heated to 30°C to adjust pH=4.0; fast feed in parallel flow, feed speed control is based on pH=3.0. After the feeding was completed, the temperature was raised to 60° C., and aged for 2.0 hours. The aging process is NH 3 ·H 2 O and HCl were used to adjust the pH to 3.0, and the stirring speed was controlled at 150 rpm during the feeding and aging process. After aging, filter and wash the powder with hot water until the anions cannot be detected. After drying, 37.64g of lanthanum iron oxalate precursor powder La 2 (C 2 o 4 ) 3 9H 2 O and FeC 2 o 4 2H 2 O.

[0026] The obtained lanthanum iron oxalate precursor powder was calcined in an air atmosphere at a temperature of 810 ° C for 6 hours to obtain 16.86 g of the precursor La 2 Fe 17 o 28.5 , and then place...

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Abstract

A coprecipitation-reduction and diffusion preparation method of ultrafine rare earth-iron-based magnetic alloy powder comprises the following steps: (1) mixing soluble rare earth chloride with 0.01 to 1.0mol/L or sulfate solution and iron chloride with 0.1 to 2.0mol/L or sulfate solution at the room temperature, heating to 25 to 35 DEG C, adjusting the pH value to 1.0 to 3.0; (2) carrying out the co-current mixing of the mixed solution of the rare earth chloride or the sulfate and the iron chloride or the sulfate which is heated to 25 to 35 DEG C and has the pH value of 1.0 to 3.0 and oxalic acid or ammonium oxalate solution which is preheated to 28 to 32 DEG C and has the pH of 1.5 to 4.5 and the concentration of 0.1mol/L to saturated concentration and adding into a stirring reactor; (3) aging; (4) filtering, precipitating and washing with hot water; (5) drying; (6) calcination; (7) pre-reduction; (8) reduction and diffusion alloying. The usage of the invention for the preparation of the ultrafine rare earth-iron-based magnetic alloy powder has low production cost, the product has small particle size, even distribution, nearly spherical or block-shaped particles and smooth surface, so the preparation method can be used for preparing the magnetic materials with good magnetic properties.

Description

technical field [0001] The invention relates to a method for preparing a permanent magnet material, in particular to a method for preparing ultrafine rare earth-iron magnetic alloy powder by chemical uniform co-precipitation-reduction diffusion. Background technique [0002] At present, the methods for preparing rare earth-iron-series metal alloys include smelting method, rapid quenching method, and reduction diffusion method. Among them, the smelting method and the quick quenching method both use simple metal as the raw material, the production cost is high, and strong ball milling is required, so it is difficult to control the size of the alloy grain and maintain the integrity of the grain. The most commonly used method is the reduction diffusion method, such as the methods disclosed in documents such as CN86100769A, CN1035700C, JP-A5-148517, they all are the mixture of oxides of rare earth metals, transition metal powder and metal calcium, under inert atmosphere. Reducti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/16B22F9/22
Inventor 郭学益薛平田庆华李栋宋瑜
Owner CENT SOUTH UNIV
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