CN104445435A - Preparation method of monodispersity superparamagnetism Fe3O4 nano-particles - Google Patents

Preparation method of monodispersity superparamagnetism Fe3O4 nano-particles Download PDF

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Publication number
CN104445435A
CN104445435A CN201410641542.7A CN201410641542A CN104445435A CN 104445435 A CN104445435 A CN 104445435A CN 201410641542 A CN201410641542 A CN 201410641542A CN 104445435 A CN104445435 A CN 104445435A
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nanoparticle
preparation
particles
monodispersity
fecl
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CN201410641542.7A
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杨景海
邹平
杨丽丽
曹健
孔祥旺
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Jilin Normal University
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Jilin Normal University
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Abstract

The invention discloses a preparation method of monodispersity superparamagnetism Fe3O4 nano-particles, and belongs to the technical field of preparation of nano-particles. The monodispersity superparamagnetism Fe3O4 nano-particles are prepared by using a chemical coprecipitation process and are prepared by adding CTAB (cetyltrimethyl ammonium bromide) and NH3.H2O into raw materials of FeCl2.4H2O and FeCl3.6H2O, and stirring for reaction. Because a surfactant namely CTAB is added, the Fe3O4 nano-particles have good monodispersity and superparamagnetism and are in the shape of particles, and the average diameter is about 10nm; and moreover, the method is simple in process, low in reaction temperature and low in cost, so that the method is favorable for large-scale production.

Description

A kind of monodisperse superparamagnetic Fe 3o 4the preparation method of nanoparticle
Technical field
The invention belongs to technical field prepared by nanoparticle, relate to a kind of chemical coprecipitation and prepare monodispersity superparamagnetism Fe 3o 4the method of nanoparticle.
Background technology
Magnetic Nano material is in sewage disposal, and medicament transport, tissue repair, the fields such as nuclear magnetic resonance are with a wide range of applications.In numerous magneticsubstance, Fe 3o 4he γ ?Fe 2o 3get more and more people's extensive concerning because magnetic property is good and toxicity is low.But, Fe 3o 4nanoparticle specific surface area is little, and itself has magnetic, and therefore agglomeration is serious, and nearly all preparation Fe 3o 4the method of nanoparticle, experiment condition is all very harsh, and working method is complicated, and cost is high, is unfavorable for scale operation.The people such as O.M.Lemine adopted sol-gel method to prepare Fe under ethanol (EtOH) super critical condition in 2012 3o 4nanoparticle, complicated operation, and agglomeration serious (Superlattices and Microstructures 52 (2012) 793 ?799).The people such as the little cranes of Central South University Liu in 2009 apply for a patent (application number: 200910043152.9), mixed system is formed with lipid acid, aliphatic amide and organic solvent, with organo-metallic molysite for raw material, utilize solvent-thermal method, at 200 DEG C ~ 280 DEG C, prepare single dispersing FE3O4 nanoparticle.Shanghai Communications University Dou Hong waits people quietly and applies for a patent (application number 201210306212.3), take high boiling organic solvent as solvent, and oleic acid is part, and high temperature thermal decomposition iron oleate obtains monodispersed oil soluble Fe 3o 4nano particle; Then the method for ligand exchange is adopted, with many carboxyls organic molecule displacement oil soluble Fe 3o 4the oleic acid ligand of nano grain surface, obtains water miscible Fe 3o 4nano particle.Reaction whole process needs protection of inert gas, and temperature of reaction is 280 DEG C ~ 380 DEG C.Although method solves Fe described in above-mentioned patent 3o 4nanoparticle agglomerates problem, but operating process is loaded down with trivial details, and cost is high.Therefore, the invention discloses a kind of coprecipitation method and prepare monodisperse superparamagnetic Fe 3o 4the method of nanoparticle, adds cetyl trimethylammonium bromide (Hexadecyl trimethyl ammonium Bromide, be called for short CTAB) in building-up process, achieves that cost is low, operating process is simple, monodispersed Fe 3o 4the preparation of nanoparticle.
Summary of the invention
The object of this invention is to provide a kind of monodisperse superparamagnetic Fe 3o 4the preparation method of nanoparticle; In building-up process, add cetyl trimethylammonium bromide (CTAB), achieve that cost is low, operating process is simple, monodispersed Fe 3o 4the preparation of nanoparticle.
The concrete technical scheme of the present invention is as follows.
A kind of monodisperse superparamagnetic Fe 3o 4the preparation method of nanoparticle, first by the FeCl of molar ratio 1: 1.8 ~ 2 24H 2o and FeCl 36H 2o is dissolved in deionized water, is stirred to solution clarification; Be added to by cetyl trimethylammonium bromide in solution, cetyl trimethylammonium bromide add-on is FeCl by mass 24H 20.33 ~ 1.01 times of O, stirs 5 minutes; Add the NH that mass concentration is 20% again 3h 2o solution, NH 3h 2the add-on of O solution is by every gram of FeCl 24H 2o adds 335 ~ 339ml and calculates; Stirring reaction 30 ~ 60min at steady temperature 40 ~ 80 DEG C; Last cool to room temperature, washes with water respectively, ethanol washes, to removing unnecessary cetyl trimethylammonium bromide.
Preferred cetyl trimethylammonium bromide add-on is FeCl by mass 24H 20.67 times of O, can obtain the Fe that monodispersity is best 3o 4nanoparticle.
Stirring reaction 40min at steady temperature 60 DEG C, just can obtain the good Fe of monodispersity 3o 4nanoparticle.
Technical characterstic of the present invention: in the past prepared Fe 3o 4during nanoparticle, in order to ensure Fe 3o 4the dispersiveness of nanoparticle, people need to use N usually 2or Ar does protection gas, and at high temperature prepare, experiment condition is harsh, and working method is complicated, and cost is high, is unfavorable for scale operation.And utilize chemical coprecipitation, add ctab surface promoting agent, effectively can realize superparamagnetism Fe 3o 4nanoparticle but dispersion, and the method is simple to operate, and temperature of reaction is low, cost is low, is beneficial to scale operation.
Beneficial effect of the present invention: adopt chemical coprecipitation, be tensio-active agent with CTAB, prepared single dispersing paramagnetism Fe 3o 4nanoparticle.Because CTAB is cationic surfactant, the existence of CTAB effectively can overcome Fe 3o 4interaction between nanoparticle, thus reach the good effect of monodispersity; And Fe 3o 4nanoparticle has superparamagnetism, and shape is particulate state, and diameter is on average at about 10nm; Method of the present invention is simple to operate, and temperature of reaction is low, cost is low, is beneficial to scale operation.
Accompanying drawing explanation
Single dispersing Fe prepared by Fig. 1 the present invention 3o 4transmission electron microscope (TEM) figure of nanoparticle.
Single dispersing Fe prepared by Fig. 2 the present invention 3o 4the magnetzation curve (VSM) of nanoparticle.
Embodiment
Embodiment 1
Concrete step of preparation process is as follows
1. medicine dissolves, and is specially: the FeCl getting 0.59654g 24H 2the FeCl of O and 1.62174g 36H 2o (FeCl 24H 2o and FeCl 36H 2the molar ratio of O is 1: 2) be dissolved in deionized water, mechanical stirring is to dissolving completely, and solution is clarified; The CTAB of 0.4g is added in the beaker of above-mentioned solution, stirs 5 minutes.
2. medicine reaction, is specially: be the NH of 20% by mass concentration 3h 2o solution 200ml be added to step 1. in, stir certain hour under steady temperature.
3. wash sample, be specially: cool to room temperature, wash with water respectively, ethanol is washed repeatedly.
Above-mentioned step 2. in, steady temperature is 60 DEG C, and certain hour is 40min.
Result of implementation is as follows: Fig. 1 provides prepared single dispersing Fe 3o 4the TEM figure of nanoparticle, as can be seen from Figure 1 uses Fe 3o 4nanoparticle has good monodispersity, and shape is particulate state, and diameter is on average at about 10nm.Fig. 2 provides the Fe of preparation 3o 4nanoparticle VSM figure (see CTAB ?NPs ?0.4g curve).
In the present embodiment
Embodiment 2
Raw material and preparation process, with embodiment 1, just change the consumption of CTAB into 0.2g by 0.4g.Result of implementation is Fe 3o 4nanoparticle has monodispersity.The Fe of preparation 3o 4the VSM figure of nanoparticle is as shown in CTAB ?NPs ?0.2g curve in Fig. 2.
Embodiment 3
Raw material and preparation process, with embodiment 1, just change the consumption of CTAB into 0.6g by 0.4g.Result of implementation is Fe 3o 4nanoparticle also has monodispersity.The Fe of preparation 3o 4the VSM figure of nanoparticle is as shown in CTAB ?NPs ?0.6g curve in Fig. 2.
With adding the different Fe measuring CTAB and prepare shown in Fig. 2 3o 4the VSM figure of nanoparticle.By embodiment 1,2,3 more known, the CTAB obtained ?the saturation magnetization (Ms) of NPs be followed successively by from high to low CTAB ?NPs ?0.2g, CTAB ?NPs ?0.4g, CTAB ?NPs ?0.6g.Due to CTAB ?NPs ?the monodispersity of 0.4g best, therefore, preferred technical scheme adopts the method adding 0.4g CTAB to prepare Fe 3o 4nanoparticle.
In above-described embodiment 1 ~ 3, FeCl 24H 2o can be slightly excessive, and product can be prevented in given scope to be transformed into Fe 2o 3.

Claims (3)

1. a monodisperse superparamagnetic Fe 3o 4the preparation method of nanoparticle, first by the FeCl of molar ratio 1: 1.8 ~ 2 24H 2o and FeCl 36H 2o is dissolved in deionized water, is stirred to solution clarification; Be added to by cetyl trimethylammonium bromide in solution, cetyl trimethylammonium bromide add-on is FeCl by mass 24H 20.33 ~ 1.01 times of O, stirs 5 minutes; Add the NH that mass concentration is 20% again 3h 2o solution, NH 3h 2the add-on of O solution is by every gram of FeCl 24H 2o adds 335 ~ 339ml and calculates; Stirring reaction 30 ~ 60min at steady temperature 40 ~ 80 DEG C; Last cool to room temperature, washes with water respectively, ethanol washes, to removing unnecessary cetyl trimethylammonium bromide.
2. monodisperse superparamagnetic Fe as claimed in claim 1 3o 4the preparation method of nanoparticle, is characterized in that, cetyl trimethylammonium bromide add-on is FeCl by mass 24H 20.67 times of O.
3. monodisperse superparamagnetic Fe as claimed in claim 1 or 2 3o 4the preparation method of nanoparticle, is characterized in that, stirring reaction 40min at steady temperature 60 DEG C.
CN201410641542.7A 2014-11-12 2014-11-12 Preparation method of monodispersity superparamagnetism Fe3O4 nano-particles Pending CN104445435A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104774831A (en) * 2015-04-23 2015-07-15 江南大学 Immobilization method of beta-galactosidase based on immobilized carrier
CN104829137A (en) * 2015-04-22 2015-08-12 同济大学 Preparation method of magnetic borate biological-activity glass support
CN108611057A (en) * 2018-05-16 2018-10-02 西安思源学院 A kind of exceptional hardness magnetic abrasive grain and preparation method thereof
CN112978803A (en) * 2021-02-23 2021-06-18 四川大学 Preparation method of water-soluble superparamagnetic ferroferric oxide microspheres with positively charged surfaces

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101870499A (en) * 2010-06-03 2010-10-27 四川大学 Ultrasonic vibration and in-situ coating preparation method of superparamagnetic ferroferric oxide nanoparticle
CN103803661A (en) * 2013-12-02 2014-05-21 郑惠娣 Preparation method of nanometer ferroferric oxide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101870499A (en) * 2010-06-03 2010-10-27 四川大学 Ultrasonic vibration and in-situ coating preparation method of superparamagnetic ferroferric oxide nanoparticle
CN103803661A (en) * 2013-12-02 2014-05-21 郑惠娣 Preparation method of nanometer ferroferric oxide

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829137A (en) * 2015-04-22 2015-08-12 同济大学 Preparation method of magnetic borate biological-activity glass support
CN104774831A (en) * 2015-04-23 2015-07-15 江南大学 Immobilization method of beta-galactosidase based on immobilized carrier
CN108611057A (en) * 2018-05-16 2018-10-02 西安思源学院 A kind of exceptional hardness magnetic abrasive grain and preparation method thereof
CN112978803A (en) * 2021-02-23 2021-06-18 四川大学 Preparation method of water-soluble superparamagnetic ferroferric oxide microspheres with positively charged surfaces

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Application publication date: 20150325