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Method for preparing superfine/nano iron oxide/iron powder

A nano iron oxide and iron powder technology, applied in the field of powder metallurgy, can solve the problems of being difficult to apply to industrial production, low output, long process, etc., and achieve the effects of easy process control, large powder output and simple process

Inactive Publication Date: 2005-12-21
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The wet method mostly uses industrial vitriol, industrial ferrous chloride and ferric nitrate as raw materials, and is prepared by oxidation precipitation method, hydrothermal method, forced hydrolysis method, colloidal chemical method, etc., and its characteristic is that the raw materials are easy to obtain and can be used directly (only Appropriate purification treatment is required), the particles are controllable, but the process is too long, the output is low, the requirements for the operating environment are strict, and the production cost is high, so it is difficult to apply to industrial production
The dry method often uses carbonyl iron (Fe(CO) 5 ) or ferrocene (FeCP 2 ) as raw material, prepared by flame thermal decomposition, low-temperature plasma chemical vapor deposition (PCVP) or laser thermal decomposition method, has the advantages of short process flow, good operating environment, high product quality, ultra-fine and uniform particles, good dispersibility, etc., but At the same time, its technical difficulty is high, the structure and material requirements of the equipment are high, and the one-time investment is large, so there is little domestic research on it.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0020] Weigh 100gFe(NO 3 ) 3 9H 2 O dissolved in 500gH 2 O;

[0021] Add 120ml of ammonia water with a concentration of 2.4wt%, and heat to 70°C to form Fe(OH) 3 colloid;

[0022] in Fe(OH) 3 Add 0.5% N, N-dimethylformamide to the colloid, and ultrasonically vibrate for 20 minutes;

[0023] Spray-dry the above-mentioned colloid to obtain an amorphous / microcrystalline nano-mixed powder precursor;

[0024] The amorphous / microcrystalline nano-mixed powder precursor is calcined at a calcination temperature of 350°C to obtain ultrafine / nanometer Fe 2 o 3 powder;

[0025] For ultrafine / nano Fe 2 O powder is ball milled to further refine its particle size to below 100nm;

[0026] The powder precursor or Fe 2 o 3 powder in H 2 Reduction under atmosphere, the reduction temperature is 500°C, and ultrafine Fe powder is further obtained.

example 2

[0028] (1) Weigh 100gFe(NO 3 ) 3 9H 2 O and 50gFeS 4 ·7H 2 O, dissolve it in 600gH 2 O;

[0029] (2) adding concentration is 2.4% ammoniacal liquor 300ml, temperature is controlled at 40 ℃;

[0030] (3) Add 0.5% polyethylene glycol, 0.1% urea and 0.05% Cr 2 o 3 , after ultrasonic vibration for 30min;

[0031] (4) spray drying the transparent colloid to obtain an amorphous or microcrystalline nano-mixed powder precursor;

[0032] (5) The powder precursor is calcined at 600°C O 2 Calcined in air atmosphere,. Get Ultrafine / Nano Fe 3 o 4 powder;

[0033] (6) The powder precursor or nanoscale Fe 2 o 3 The powder is reduced at a temperature of 400°C in a hydrocarbon gas mixture to obtain ultra-fine Fe powder.

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PUM

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Abstract

The invention relates to the powder metallurgy domain, specially used in the preparation method of nano / superfine ferric oxide. Tts characteristic lies in: Uses Fe(NO)3 the crystal (Fe (NO3) 3 - 9H2O), the ferrous sulfate crystal (FecSO4 - 7H2O), the ferric chloride crystal (FeCl3 - 6H2O) as the raw material, which matches the density - 30wt% molysite solution; Joins the ammonia water and adjusts pH to 1.5-3; Then joins 0.1-1.0% surface active agent and 0.01-0.1% crystal grain inhibitor, vibrates 10 - 60min after the ultrasonic waving, obtains the transparent colloid; Then dry, then gets the superfine mix powder forerunner body; Under 350 - 700 íµ temperatures for calcination, then obtains the nanometer / superfine ferric oxide powder. This invention preparation powder granularity is thin, which is smaller than 100nm, high purity which can reaches 99% - 99.5%, which is serviceable and makes the high performance magnetic powder and the absorbing material; The craft is simple, the process is easy to control, the powder output is high.

Description

Technical field: [0001] The invention relates to the field of powder metallurgy, in particular to a method for preparing ultrafine / nanometer iron oxide by adopting nanotechnology. Background technique: [0002] Nano-iron oxide preparation methods can be generally divided into wet method (Wet Method) and dry method (Dry Method). The wet method mostly uses industrial vitriol, industrial ferrous chloride and ferric nitrate as raw materials, and is prepared by oxidation precipitation method, hydrothermal method, forced hydrolysis method, colloidal chemical method, etc., and its characteristic is that the raw materials are easy to obtain and can be used directly (only Appropriate purification treatment is required), and the particles are controllable, but the process is too long, the output is low, the requirements for the operating environment are strict, and the production cost is high, so it is difficult to apply to industrial production. The dry method often uses carbonyl ir...

Claims

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Application Information

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IPC IPC(8): C01G49/06
Inventor 范景莲成会朝
Owner CENT SOUTH UNIV
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