CN102097194A - Method for preparing core-shell structured SiO2/Fe3O4 compound magnetic particle - Google Patents
Method for preparing core-shell structured SiO2/Fe3O4 compound magnetic particle Download PDFInfo
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- CN102097194A CN102097194A CN 201010583415 CN201010583415A CN102097194A CN 102097194 A CN102097194 A CN 102097194A CN 201010583415 CN201010583415 CN 201010583415 CN 201010583415 A CN201010583415 A CN 201010583415A CN 102097194 A CN102097194 A CN 102097194A
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Abstract
The invention discloses a method for preparing a core-shell structured SiO2/Fe3O4 magnetic particle. The core-shell structured SiO2/Fe3O4 magnetic particle is characterized in that Fe3O4 is used as the magnetic core and SiO2 is used as the shell to form the SiO2/Fe3O4 core-shell covering structure. The method comprises the following steps: under the heat condition of a solvent glycol, taking ferric chloride as the Fe source, sodium acetate as a reducing agent and a right amount of polyethylene glycol as a dispersing agent, heating the system to 150-180 DEG C and then preserving heat for several hours; and after washing and drying, mixing the synthesized Fe3O4 powder with a right amount of absolute ethyl alcohol, deionized water and surfactants, dropwise adding a certain amount of stronger ammonia water, after ultrasonic dispersion, slowly dropwise adding tetraethoxysilane under the condition of stirring, continuing stirring for reaction for several hours and then washing and drying the product, thus obtaining the SiO2/Fe3O4 compound particle. The method has the following advantages: the process is simple; the cost is low; the reaction conditions are easy to control; the core-shell structured SiO2/Fe3O4 magnetic particle can be produced in a large scale; and therefore, the method has a good application prospect.
Description
Technical field
The present invention relates to a kind of core-shell structure SiO that uses as magnetic carrier
2/ Fe
3O
4The preparation method of particle belongs to the nano material preparing technical field.
Technical background
Magnetic Fe
3O
4Microballoon is as a kind of novel functional material, has good magnetic performance, such as superparamagnetism and high saturation and magnetic intensity etc., all having broad application prospects as aspects such as magnetic recording material, magnetic liquid, sensor, catalyst carrier, permanent-magnet material, pigment, radar absorbing materials.But because magnetic nano-particle has higher specific area and strong gathering tendency, and chemical stability is not high, and is easily oxidized, is difficult to direct application.In order to address these problems, must to carry out finishing to magnetic nano-particle and make its stabilisation.In recent years, inorganic material SiO
2Be subjected to people and pay close attention to greatly because having the advantages such as good biocompatibility, hydrophily and chemical inertness and colloidal stability, be used to modify various materials, comprise magnetic Fe
3O
4
At present, synthetic SiO
2/ Fe
3O
4The method of composite magnetic nano particle mainly contains microemulsion method and sol-gel process.The SiO of microemulsion method preparation
2/ Fe
3O
4The magnetic coupling particle size is even, and is better dispersed, but is subjected to the restriction of microemulsion system stability, the adjustable particle size of synthetic magnetic coupling particle is limited in scope, and microemulsion system is very sensitive to preparation temperature and change of component, and experimental repeatability is bad, output is little, is difficult to large-scale production; And sol-gel process is because technology is simple, environmental friendliness and advantage that can large-scale production and extremely people's favor, but the pattern of the magnetic core that the structure of the composite magnetic particle that this method obtains and pattern are prepared easily and the impact of particle diameter, the preparation technology that original magnetic is examined has relatively high expectations.Therefore utilizing sol-gel process to forming SiO at present
2/ Fe
3O
4In the report of composite magnetic nano particle, because bad to the structure control of magnetic parent nucleus, a lot of compound particles do not form the obvious core-shell structure of covered effect, and SiO
2Coating thickness is inhomogeneous, it is serious to reunite between the magnetic core.The present invention at first adopts solvent-thermal method to synthesize the uniform spherical Fe of particle size of high dispersive
3O
4The magnetic parent nucleus utilizes the hydrolytic process of ammoniacal liquor control ethyl orthosilicate under normal temperature condition, the easy preferably SiO of dispersiveness that prepared
2/ Fe
3O
4Shell is examined clad structure magnetic coupling particle, and can regulate SiO by the consumption that changes ammoniacal liquor
2The thickness of shell.
Summary of the invention
The purpose of this invention is to provide a kind of simple to operate, mild condition, the obvious SiO of shell nuclear clad structure
2/ Fe
3O
4The preparation method of magnetic compound particles.
Concrete steps of the present invention are as follows:
(1) with a certain amount of ethylene glycol as solvent, with iron chloride, sodium acetate is dissolved in the ethylene glycol, add again an amount of polyethylene glycol continuation stirring under the magnetic force high-speed stirred condition and obtain mixed liquor, pour into then in the autoclave, be heated to seal to uniform temperature and be incubated a few hours, washing is put oven drying and is namely got black Fe then
3O
4Powder.
The volume ratio of the shared reactor of described adding ethylene glycol is 0.4-0.8.
(2). under the room temperature, with absolute ethyl alcohol, deionized water, above-mentioned Fe
3O
4Powder, a certain amount of surfactant mixes, and adds an amount of concentrated ammonia liquor, and ultrasonic dispersion drips ethyl orthosilicate slowly under the stirring condition, continue stirred for several hour, with product washing and dry, can obtain SiO
2/ Fe
3O
4Composite magnetic particle.Described surfactant is: neopelex, softex kw, 4-propyl bromide, TBAB.
It is described that to add the volume ratio that concentrated ammonia liquor accounts for ethanol water be 0.2-2%.
Have the following advantages according to preparation method of the present invention:
(1). the Fe of the present invention's preparation
3O
4Magnetic parent nucleus uniform particles, good dispersion, and can produce in batches.
(2). preparation method of the present invention is simple to operate, mild condition, cost are low, synthetic SiO
2/ Fe
3O
4The core-shell structure of magnetic compound particles is clear, and composite particles presents obvious polymolecularity, and can regulate SiO by the consumption that changes ammoniacal liquor
2The thickness of shell.
Description of drawings:
The Fe of Fig. 1: embodiment 1
3O
4Particle TEM photo
The SiO of Fig. 2: embodiment 1
2/ Fe
3O
4Core-shell structure particle TEM photo
The SiO of Fig. 3: embodiment 3
2/ Fe
3O
4Core-shell structure particle TEM photo
Embodiment
(1) ethylene glycol of measuring 112ml is as solvent, and with 3.78g iron chloride, the 10.08g sodium acetate is dissolved in the ethylene glycol, and magnetic force high-speed stirred 10 minutes adds an amount of polyethylene glycol (molecular weight 1500) continuation stirring again and obtains mixed liquor after 30 minutes.Poured into then in the teflon-lined autoclave, inserted in the baking oven after the reactor sealing, be heated to 180 ℃ after insulation 9 hours.To three pH=7 to solution of washing of precipitate, use again the ethanol washed twice with deionized water, put in the baking oven in 60 ℃ of dryings 6 hours, namely get black Fe
3O
4Powder.
Synthetic Fe
3O
4Parent nucleus is seen Fig. 1, and particle diameter is about 400nm.
(2) under the room temperature, with the 90ml absolute ethyl alcohol, 22.5ml deionized water, the above-mentioned Fe of 0.3g
3O
4Powder, the 0.5g neopelex mixes, and drips then the 0.63ml concentrated ammonia liquor, and ultrasonic dispersion slowly dripped the 1ml ethyl orthosilicate after 30 minutes under the stirring condition, continue stirring reaction 6h, the same step washing, 60 ℃ of dryings can obtain SiO then
2/ Fe
3O
4Compound particle
Synthetic SiO
2/ Fe
3O
4The core-shell structure particle is seen Fig. 2, SiO
2The thickness of shell is about 100nm.
Embodiment 2
The consumption that changes concentrated ammonia liquor is 0.315ml, and other drug dosage and operating procedure are with embodiment 1.
Embodiment 3
The consumption that changes concentrated ammonia liquor is 1.26ml, and other drug dosage and operating procedure are with embodiment 1.
Synthetic SiO
2/ Fe
3O
4The core-shell structure particle is seen Fig. 3, SiO
2The thickness of shell is about 40nm.
Embodiment 4
The consumption that changes concentrated ammonia liquor is 1.89ml, and other drug dosage and operating procedure are with embodiment 1.
Embodiment 5
Change surfactant, select neopelex in the softex kw alternative embodiment 1 for use, other operating procedure is with embodiment 1.
Embodiment 6
Change surfactant, select neopelex in the 4-propyl bromide alternative embodiment 1 for use, other operating procedure is with embodiment 1.
Embodiment 7
Change surfactant, select neopelex in the TBAB alternative embodiment 1 for use, other operating procedure is with embodiment 1.
Claims (5)
1. core-shell structure SiO who uses as magnetic carrier
2/ Fe
3O
4Particle is characterized in that its structural group becomes: Fe
3O
4Be magnetic core, SiO
2Be the inertia shell, form shell nuclear clad structure.
2. core-shell structure SiO according to claim 1
2/ Fe
3O
4The preparation method of particle is characterized in that, this method may further comprise the steps:
(1) take ethylene glycol as solvent, iron chloride is source of iron, and sodium acetate is reducing agent, and polyethylene glycol is dispersant, pours in the autoclave (0.2-1.0L) after evenly mixing, and is incubated 5-12h after being heated to 150-200 ℃ after the sealing.Namely get black Fe after the product washing drying
3O
4Powder.
(2) under the room temperature with an amount of ethanol water and the Fe that makes
3O
4Powder and proper amount of surfactant are mixed, and add concentrated ammonia liquor as precipitating reagent, drip the 0.1-3.0ml ethyl orthosilicate under the stirring condition, and reaction 1-10h obtains SiO after the product washing drying
2/ Fe
3O
4The core-shell structure compound particle.
3. preparation method according to claim 2 is characterized in that, the volume ratio that adds the shared reactor of ethylene glycol is 0.4-0.8.
4. preparation method according to claim 2 is characterized in that, to add the volume ratio that concentrated ammonia liquor accounts for ethanol water be 0.2-2%.
5. preparation method according to claim 2 is characterized in that, used surfactant is neopelex, softex kw, 4-propyl bromide, TBAB.
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| CN 201010583415 CN102097194A (en) | 2010-12-10 | 2010-12-10 | Method for preparing core-shell structured SiO2/Fe3O4 compound magnetic particle |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010583415 CN102097194A (en) | 2010-12-10 | 2010-12-10 | Method for preparing core-shell structured SiO2/Fe3O4 compound magnetic particle |
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| Publication Number | Publication Date |
|---|---|
| CN102097194A true CN102097194A (en) | 2011-06-15 |
Family
ID=44130242
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|---|---|---|---|
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Application publication date: 20110615 |