CN100567169C - A kind of ferromagnetic gamma Fe 2O 3The preparation method of powder - Google Patents

A kind of ferromagnetic gamma Fe 2O 3The preparation method of powder Download PDF

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CN100567169C
CN100567169C CNB2007101868806A CN200710186880A CN100567169C CN 100567169 C CN100567169 C CN 100567169C CN B2007101868806 A CNB2007101868806 A CN B2007101868806A CN 200710186880 A CN200710186880 A CN 200710186880A CN 100567169 C CN100567169 C CN 100567169C
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powder
preparation
ferromagnetic
gamma
ferromagnetic gamma
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CN101172662A (en
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长山
赵斯琴
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Inner Mongolia Normal University
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Abstract

The invention discloses a kind of ferromagnetic gamma Fe 2O 3The preparation method of powder, this method directly go out γ Fe from the urea complex preparation of iron 2O 3Powder.The granularity controlled range of powder is that its saturation magnetization can reach 73emu/g from several nanometers to tens micron, with aciculiform γ Fe 2O 3Substantially consistent.With traditional γ Fe 2O 3Powder preparation method is compared, and the simple one-step synthesis of this technology does not need complicated equipment, and cost is low.

Description

A kind of ferromagnetic gamma Fe 2O 3The preparation method of powder
Technical field
The present invention relates to a kind of Fe 2O 3The preparation method of powder refers in particular to a kind of ferromagnetic gamma Fe 2O 3The preparation method of powder.
Background technology
Ferromagnetic gamma Fe 2O 3Powder is quite extensive in the application in following field: 1, be applied to various sound carriers (magnetic storage) as tape; 2, be applied to electronics and photoelectron product (electronicsand optoelectronics); 3, be applied to biologic medical (biomedical) aspect: (a) cellular segregation (cell separation); (b) protein purification (protein purification); (c) immunoassay (immunoassays).Traditional ferromagnetic gamma Fe that is used for tape, magnetic fluid 2O 3The preparation method of powder is very complicated, and it just can obtain by following six steps:
1, contains that the hydro-oxidation sodium solution prepares Fe (OH) in the solution of ferrous ion 2Precipitation;
2, atmospheric oxidation Fe (OH) 2Precipitation makes it change into needle-like alpha-feooh or γ-FeOOH crystal;
3,300 ℃ of calcinings needle-like alpha-feooh or γ-FeOOH crystal make it change into acicular α-Fe 2O 3Crystal;
4,600 ℃ of calcining α-Fe 2O 3Crystal;
5, at nitrogen, hydrogen, 400 ℃ of calcinings (reduction) α-Fe in the mist of steam 2O 3Crystal makes it change into needle-like Fe 3O 4
6,300 ℃ of calcinings (oxidation) needle-like Fe in air 3O 4, make it change into needle-like γ Fe 2O 3
From the above-mentioned shortcoming of finding out the traditional preparation process method: 1, the needed step of technology is too complicated; 2, because from ferrous ion, institute thinks control reaction needed air-isolation (logical usually nitrogen).
Summary of the invention
The technical problem to be solved in the present invention provides a kind of ferromagnetic gamma Fe 2O 3The preparation method of powder, this method device therefor is simple, cost is low, can a step obtain γ Fe 2O 3Powder.The another one characteristics are that the urea title complex and the raw material thereof of iron is all nontoxic, all are common chemical feedstockss.
The technical problem to be solved in the present invention is realized by following scheme:
A kind of ferromagnetic gamma Fe 2O 3The preparation method of powder is characterized in that: with the urea complex [Fe (CON of iron 2H 4) 6] (NO 3) 3100 ℃~300 ℃ heating flames just obtain γ Fe in air 2O 3Powder.
Advantage of the present invention is: this method directly goes out γ Fe from the urea complex preparation of iron 2O 3Powder.The granularity controlled range of powder is that its saturation magnetization can reach 73emu/g from several nanometers to tens micron, with aciculiform γ Fe 2O 3Substantially consistent.With traditional γ Fe 2O 3Powder preparation method is compared, and this preparation method one-step synthesis is fairly simple, does not need complicated equipment, and cost is low.
Description of drawings
Fig. 1 is with [Fe (CON 2H 4) 6] (NO 3) 3200 ℃ are heated the x-ray diffraction pattern that obtained powder in 1 hour in air.Table 1 is the contrast that records spacing value (d) and JCPD standard card.Can find out, obtain data and γ Fe 2O 3Standard card basically identical, and be different from Fe 3O 4Standard card.As shown in Figure 1, table 1 is the contrast of d value and standard card
Figure C20071018688000041
a:JCPDS?file?No.39-1346
b:JCPDS?file?No.19-629
Fig. 2 is with [Fe (CON 2H 4) 6] (NO 3) 3200 ℃ are heated the hysteresis curve (M-H curve) that obtained powder in 1 hour in air.This result shows, obtains the feature that powder has strong magnetic material.Its saturation magnetization (Ms) is 67.45emu/g, and coercivity (Hc) is 212Oe, and remanent magnetism (Mr) is 16.82emu/g.
Embodiment
One embodiment is described in detail in detail below: in the organic solvents such as ethanol with urea (CON 2H 4) and Fe 3+Soluble inorganic salt such as ferric nitrate, can obtain absinthe-green [Fe (CON by 1: 6 mixed in molar ratio 2H 4) 6] (NO 3) 3Crystal powder;
Reaction equation: Fe 3++ 6CON 2H 4+ 3NO 3 -→ [Fe (CON 2H 4) 6] (NO 3) 3.
Get 20g ferric nitrate (Fe (NO 3) 39H 2O) under the magnetic agitation condition, be dissolved in the 40mL absolute ethyl alcohol, add again 20g urea (CON 2H 4), continue to stir 3 hours, generate a large amount of light green precipitation urea iron complexes, normal pressure filters and with absolute ethanol washing for several times, naturally dries, and obtains the light green powder.Get this powder of 5g in crucible, and put in the electric furnace, the programming rate with 10 ℃/minute in air is warming up to 200 ℃, continues heating and just obtains γ Fe in 1 hour 2O 3Powder.

Claims (1)

1, a kind of ferromagnetic gamma Fe 2O 3The preparation method of powder is characterized in that: with the urea complex [Fe (CON of iron 2H 4) 6] (NO 3) 3100 ℃~300 ℃ heating flames just obtain γ Fe in air 2O 3Powder.
CNB2007101868806A 2007-11-20 2007-11-20 A kind of ferromagnetic gamma Fe 2O 3The preparation method of powder Expired - Fee Related CN100567169C (en)

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