CN101357779B - Method for preparing nano Fe3O4 powder - Google Patents
Method for preparing nano Fe3O4 powder Download PDFInfo
- Publication number
- CN101357779B CN101357779B CN2008101459141A CN200810145914A CN101357779B CN 101357779 B CN101357779 B CN 101357779B CN 2008101459141 A CN2008101459141 A CN 2008101459141A CN 200810145914 A CN200810145914 A CN 200810145914A CN 101357779 B CN101357779 B CN 101357779B
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- powder
- nanometer
- ferric
- fe3o4 powder
- preparation
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Abstract
The invention discloses a preparation method of nanometer Fe3O4 powder and provides a technological process that absolute ethyl alcohol and ferric urea composition (Fe(CON2H4)6) (NO3)3 are added into a high-pressure reactor vessel lined with polytetrafluoroethylene with the mass ratio of 1:10 to 100 and react with each other in the vessel; then the absolute ethyl alcohol and the ferric urea composition are put into an electric oven in which the temperature rises from 150 to 250 DEG C with the heating rate of 5 to 15 DEG C per minute and black precipitates are obtained after the absolute ethylalcohol and composition are continuously heated for 10 to 50 hours under the temperature of 150 to 250 DEG C; black nanometer Fe3O4 powder is obtained through the filtration and air drying of the precipitates. The method directly prepares the nanometer Fe3O4 powder from the ferric urea composition and the particle size is controlled within the range of a plurality of nanometers to dozens of nanometers. The characteristic results of magnetic properties show that the powder has super para-magnetism. Compared with a traditional preparation method of the nanometer Fe3O4 powder, the process has simple synthesis with one step and can prepare mono-disperse nanometer Fe3O4 powder, the particle size of which can be controlled.
Description
Technical field
The present invention relates to a kind of Fe
3O
4The preparation method of powder refers in particular to a kind of nanometer Fe
3O
4The preparation method of powder.
Background technology
At present, Fe
3O
4Powder is quite extensive in the application in following field: 1, recording materials; 2, pigment; 3, magnetic fluid material; 4, catalyzer; 5, electronic material.In addition, Fe
3O
4Powder also has a wide range of applications at biological technical field and medical domain, and employed such as target delivery system in the oncotherapy is exactly super-paramagnetism nano Fe
3O
4Powder.
Preparation Fe
3O
4The method of powder can be divided into solid phase method and liquid phase method two big classes generally.Solid phase method mainly comprises thermal decomposition method and arc plasma process etc.; And liquid phase method mainly comprises the precipitator method, hydrothermal method (solvent-thermal method), sol-gel method, electrochemical process and microemulsion method etc.Wherein hydrothermal method (solvent-thermal method) is a kind of preparation method that latest developments are got up.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of nanometer Fe
3O
4The preparation method of powder, this method technology is simple, can a step obtain nanometer Fe
3O
4Powder.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 nanometer Fe
3O
4The preparation method of powder is characterized in that: with the urea complex [Fe (CON of iron
2H
4)
6] (NO
3)
3With absolute ethyl alcohol with 1: the weight ratio of 10-100 is put into the polytetrafluoroethyllining lining autoclave and is reacted, put into together in the Electric heat oven again, be warming up to 150 ℃-250 ℃ with 5 ℃-15 ℃/minute programming rates, continuous heating obtained black precipitate in 10 hours-50 hours under this temperature, then sediment was filtered to dry just to obtain black nano Fe
3O
4Powder.
Advantage of the present invention is: this method directly goes out nanometer Fe from the urea complex preparation of iron
3O
4Powder.By changing reaction condition, can prepare the dispersed nano Fe of different size
3O
4Powder, the granularity controlled range is from several nanometers to tens nanometer.With traditional Fe
3O
4Powder preparation method is compared, and this preparation method can prepare the controlled dispersed nano Fe of particle size
3O
4Powder.
Description of drawings
Fig. 1 is the preparation nanometer Fe
3O
4The process chart of powder.
Fig. 2 is with [Fe (CON
2H
4)
6] (NO
3)
3And C
2H
5OH 200 ℃ of heating in autoclave obtained the x-ray diffraction pattern of powder in 30 hours.
Fig. 3 is with [Fe (CON
2H
4)
6] (NO
3)
3And C
2H
5OH 200 ℃ of heating in autoclave obtained the room temperature hysteresis curve (M-H curve) of powder in 30 hours.This result shows, obtains the feature that powder has superparamagnetic material, and its coercivity (Hc) and remanent magnetism (Mr) are zero.
Fig. 4 is the contrast that records spacing value (d) and JCPD standard card.Can find out, obtain data and Fe
3O
4Standard card basically identical, and be different from γ-Fe
2O
3Standard card.
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 1g and 20g dehydrated alcohol in the polytetrafluoroethyllining lining autoclave, and put in the Electric heat oven, be warming up to 200 ℃, continue heating and obtained black precipitate in 30 hours with 10 ℃/minute heat-up rates.Then sedimentation and filtration is dried and just obtain black Fe
3O
4Powder.
Claims (1)
1. nanometer Fe
3O
4The preparation method of powder is characterized in that: with the urea complex [Fe (CON of iron
2H
4)
6] (NO
3)
3With absolute ethyl alcohol with 1: the weight ratio of 10-100 is put into the polytetrafluoroethyllining lining autoclave and is reacted, put into together in the Electric heat oven again, be warming up to 150 ℃-250 ℃ with 5 ℃-15 ℃/minute programming rates, continuous heating obtained black precipitate in 10 hours-50 hours under this temperature, then sediment was filtered to dry just to obtain black nano Fe
3O
4Powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101459141A CN101357779B (en) | 2008-08-07 | 2008-08-07 | Method for preparing nano Fe3O4 powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101459141A CN101357779B (en) | 2008-08-07 | 2008-08-07 | Method for preparing nano Fe3O4 powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101357779A CN101357779A (en) | 2009-02-04 |
| CN101357779B true CN101357779B (en) | 2010-11-10 |
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ID=40330399
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101459141A Expired - Fee Related CN101357779B (en) | 2008-08-07 | 2008-08-07 | Method for preparing nano Fe3O4 powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101357779B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515281A (en) * | 2011-11-18 | 2012-06-27 | 内蒙古师范大学 | Preparation method for Fe3O4 magnetic fluid and water-soluble Fe3O4 powder |
| CN106735287B (en) * | 2016-11-28 | 2018-08-28 | 东北大学 | A kind of monodispersed FePt/Fe3O4Mix the preparation method of nano particle |
| CN108371938A (en) * | 2018-05-09 | 2018-08-07 | 上海大学 | Mesoporous magnetic Nano iron oxide material, preparation method and applications |
| CN108786716A (en) * | 2018-06-08 | 2018-11-13 | 龙岩学院 | Fe3O4Adulterate montmorillonite composite material and its application |
| CN109231281B (en) * | 2018-08-06 | 2020-08-28 | 杭州电子科技大学 | Fe3O4Preparation method of quasi-cubic particle/multilayer graphene composite material |
-
2008
- 2008-08-07 CN CN2008101459141A patent/CN101357779B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101357779A (en) | 2009-02-04 |
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