CN102794140A - Preparation method of grain size-controllable nuclear shell Fe3O4/SiO2 nanoparticle - Google Patents

Preparation method of grain size-controllable nuclear shell Fe3O4/SiO2 nanoparticle Download PDF

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CN102794140A
CN102794140A CN2012103163798A CN201210316379A CN102794140A CN 102794140 A CN102794140 A CN 102794140A CN 2012103163798 A CN2012103163798 A CN 2012103163798A CN 201210316379 A CN201210316379 A CN 201210316379A CN 102794140 A CN102794140 A CN 102794140A
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朱利民
张培培
聂华丽
娄少锋
田利强
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Donghua University
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Abstract

The invention relates to a preparation method of a grain size-controllable nuclear shell Fe3O4/SiO2 nanoparticle, which comprises the following steps: (1) dissolving Fe3O4, cetyltrimethyl ammonium bromide and tetraethoxysilane into a solvent and carrying out ultrasonic treatment to obtain mixed solution; and then adding polyvinylpyrrolidone powder and uniformly agitating to obtain brown spinning solution; (2) carrying out electrostatic spinning by adopting the spinning solution to obtain nanofiber; and (3) putting the nanofiber into ethanol water solution and agitating at a temperature of 20-40 DEG C and at a speed of 100-500 r/min to obtain the nuclear shell Fe3O4/SiO2 nanoparticle. The preparation method has the advantages of simplicity and convenience in operation, moderate reaction condition, cheap and easily-available raw materials, no toxicity and no pollution, and excellent biological compatibility, and the nuclear shell Fe3O4/SiO2 nanoparticle obtained by the preparation method has excellent magnetic property, uniform grain size, more regular shape and high chemical stability.

Description

The nucleocapsid Fe that particle diameter is controlled 3O 4/ SiO 2The preparation method of nanoparticle
Technical field
The invention belongs to Fe 3O 4The preparation field of composite particles, the nucleocapsid Fe that particularly a kind of particle diameter is controlled 3O 4/ SiO 2The preparation method of nanoparticle.
Background technology
In recent years, magnetic nano-particle, particularly Fe 3O 4And γ-Fe 2O 3, because they have caused researcher's concern in the application of biology and biomedical aspect.These application comprise the immobilization of targeted drug transmission, Magnetic resonance imaging, magnetic mediation thermotherapy, enzyme etc.But because dipolar magnetic interaction, exposed maghemite nano particle is assembled bunchy easily to reduce their surface ability, so in water with in the organic solvent, have weak dispersiveness.In addition, because maghemite comprises Fe2+, be easy to oxidizedly, when they are exposed in the biosystem, be easy to lose magnetism, this has just limited their application.Therefore, in order to increase Fe 3O 4The dispersiveness of nano particle and non-oxidizability are carried out modification with chemically stable and material with biocompatibility to it and are coated with the surface and be very important.
Mesoporous SiO 2Have a large amount of good characteristics, comprise hypotoxicity, high surface, big pore volume, adjustable hole dimension and excellent biological compatibility.In addition, its silanol surface is easy to carry out modification with a series of functional group.Therefore, SiO 2It is the excellent material of preparation magnetic compound particles.Use SiO 2Coated magnetic nanoparticle not only can stop Fe 3O 4Reunion but also can provide a silica similarly the surface.Therefore, Fe 3O 4SiO 2Obtain extensive studies, and many technologies of preparing occurred.Up to the present; method is most popular; Because reaction condition is gentle relatively, the material of preparation process low cost and preparation is homogeneous relatively.In the period of past several, through
Figure GDA00002078900000012
Method or modification
Figure GDA00002078900000013
Legal system is equipped with Fe 3O 4SiO 2Work emerge in an endless stream.
But, the most Fe that up to the present prepares 3O 4SiO 2Material can not satisfy actual needs, or is because low Fe 3O 4The weak magnetic that causes of load capacity, or be because the size of nano particle is inadequately little.Recently, Chang etc. uses mesoporous SiO 2Parcel Fe 3O 4Nuclear has prepared magnetic nano-particle through the sol-gel process of modification, but the not enough 3emu/g of its saturation magnetization.Yang etc. have also prepared SiO through the sol-gel process of seed 2The Fe that shell is controlled 3O 4SiO 2Particle.Yet the saturation magnetization of these nano particles is also just in the scope of 3.0-15emu/g.Recently also have some other research, Deng etc., through surfactant-template method prepared sandwich structure mesoporous microsphere (～500nm).Luo etc., through modification
Figure GDA00002078900000014
Process has been synthesized nucleocapsid Fe 3O 4SiO 2Microballoon.Although these magnetic particles are quick on the draw to magnetic field, they have big relatively particle size.Therefore, be badly in need of proposing a kind of new controlled ferromagnetism Fe of tactful preparation size 3O 4SiO 2Nano particle.
Summary of the invention
Technical problem to be solved by this invention provides the controlled nucleocapsid Fe of a kind of particle diameter 3O 4/ SiO 2The preparation method of nanoparticle, this method is simple to operate, reaction condition is gentle, and raw material are cheap and easy to get, and can be to Fe 3O 4The particle diameter of/SiO2 nanoparticle is effectively controlled.
The nucleocapsid Fe that a kind of particle diameter of the present invention is controlled 3O 4/ SiO 2The preparation method of nanoparticle comprises:
(1) with Fe 3O 4, CTAB (softex kw) and TEOS (ethyl orthosilicate) be dissolved in the solvent, after the sonicated mixed solution; And then the adding polyvinylpyrrolidonepowder powder, stir, get brown spinning solution;
(2) adopt above-mentioned spinning solution to carry out electrostatic spinning, obtain nanofiber;
(3) above-mentioned nanofiber is placed ethanol water,, promptly get strong magnetic core-shell Fe at 20 ℃-40 ℃ powerful down stir (100-500r/min) 3O 4/ SiO 2Nanoparticle.
Fe described in the step (1) 3O 4, CTAB and TEOS amount ratio be 0.05-0.2g:0.1-0.2g:0.25-1.0mL.
Solvent described in the step (1) is an isopropyl alcohol.
Polyvinylpyrrolidone described in the step (1) is polyvinylpyrrolidone K90 (PVP K90), and molecular weight is 360000.
The consumption and the Fe of the polyvinylpyrrolidone described in the step (1) 3O 4Mass ratio be 0.8-1.2:0.05-0.2.
Fe in the spinning solution described in the step (1) 3O 4Concentration be 0.002-0.008g/mL.
The syringe specification of being selected for use in the electrostatic spinning described in the step (2) is 5mL, and the syringe needle internal diameter is 1mm, and receiving screen adopts the reception of aluminium foil ground connection.
The technological parameter of the electrostatic spinning described in the step (2) is: the ejection flow velocity is 2-3.5mL/h, voltage 10-13kv, and the distance of syringe needle and receiving screen is 15-18cm.
The volume ratio 80-100:20-50 of ethanol and distilled water in the ethanol water described in the step (3).
Ethanol water described in the step (3) is an alkalescent, and its pH value is 8.0-10.0.
The resulting nucleocapsid Fe of step (3) 3O 4/ SiO 2The saturation magnetization of nanoparticle is 30-50emu/g.
Change Fe in the spinning solution among the present invention 3O 4Concentration, can make the electro spinning nano fiber of different-diameter, thereby can obtain the nucleocapsid Fe of different-grain diameter 3O 4/ SiO 2Nanoparticle.
Fe of the present invention 3O 4/ SiO 2Magnetic nanoparticle not only has all advantages that superparamagnetism, water-soluble, chemical stability, biocompatibility and general nano particle are had, and there is higher magnetic responsiveness relatively in magnetic field.Believe that this magnetic nano-particle will become the star of biomedical sectors such as being applied to target medicine carrier, immobilised enzymes, cell separation, nuclear magnetic resonance, immune detection and purifying biomolecules through further surface modification.
The present invention prepares the controlled strong magnetic core-shell Fe of particle diameter through the mode of electro spinning nano fiber self assembly 3O 4/ SiO 2Nanoparticle, obtained that magnetic particle content is high, magnetic responsiveness is strong, nano particle diameter is controlled (<nucleocapsid structure compound particle 100nm) is to satisfy biomedical requirement.
It is a kind of polymer generating technique that electricity spins, and can be used to prepare the controlled 1-dimention nano fiber of secondary structure.It is the simple and the most general technology of preparation nano-scale compound.Electrospinning fibre is made up of polymer substrate, and the function compound disperses wherein.Fiber after the collection formation fibrofelt that is intertwined usually.They have good character, for example ultra-fine size, and big surface area, and fibrofelt has high hole.These character have promoted the quick dissolving of fiber, the infiltration of solute and solvent and dispersion.
In addition, electro spinning nano fiber can be used as template through secondary interaction for example hydrophobic effect power and the hydrogen bond control transportation of constructing matrix with contact, can control the molecule self assembly like this.This is extremely important, because use traditional self assembly approach, the stirring mucus is difficult in and accurately controls the transportation of constructing matrix on the molecular level in limited space.In work before, we once prepared nano particle through the self assembly of electro spinning nano fiber template-driven.And can control the size of self-assembled nanometer particle through the electrospinning fibre template.
The present invention prepares the controlled ferromagnetism Fe of particle diameter through the mode of electro spinning nano fiber self assembly 3O 4/ SiO 2The core-shell nano grain, this method is simple to operate, reaction condition is gentle, and raw material are cheap and easy to get, and can be to Fe 3O 4The particle diameter of/SiO2 nanoparticle is effectively controlled.In addition, these magnetic nano-particles are owing to having ferromagnetism, so in the application of various reality, have broad prospects.And the template action of self assembling process possibly promote the preparation of three layers or four layers more complicated core-shell nano.
Beneficial effect:
(1) of the present invention easy and simple to handle, reaction condition is gentle, employed raw material are cheap and easy to get, nontoxic pollution-free has good biocompatibility;
(2) the resulting Fe of the present invention 3O 4/ SiO 2Nanoparticle has superior magnetic performance, uniform particle diameter, and form is more regular, and chemical stability is high, also has the advantage of general nano particle simultaneously.
(3) the present invention prepares ferromagnetism Fe 3O 4/ SiO 2The method of nanoparticle can be to Fe 3O 4/ SiO 2The particle diameter of particle is effectively controlled.
Description of drawings
Fig. 1 is different Fe 3O 4The spinning solution electricity of concentration spins gained nanofiber F 1, F 2, F 3Sem photograph F 1(a), F 2(b) and F 3(c) and diameter Distribution F 1(d), F 2(e) and F 3(f);
Fig. 2 is fiber F 1, F 2, F 3The Fe that self assembly obtains 3O 4/ SiO 2Particle NP-1, NP-2, the field emission scanning electron microscope figure NP-1 (a) of NP-3, NP-2 (b) and NP-3 (c) and transmission electron microscope picture NP-1 (a) thereof, NP-2 (b) and NP-3 (c);
Fig. 3 is fibre diameter and Fe 3O 4/ SiO 2Particle diameter between relation;
Fig. 4 is Fe 3O 4(a), NP-3 (b), the XRD figure of NP-2 (c) and NP-1 (d);
Fig. 5 is Fe 3O 4(a), NP-3 (b), the hysteresis curve of NP-2 (c) and NP-1 (d).
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Press following step preparing spinning solution: with 0.05g Fe 3O 4, 0.2g CTAB and 1.0mL TEOS is dissolved separates in the Erlenmeyer flask that fills the 10mL isopropyl alcohol; Sonicated 15min afterwards; Then 1.0g PVP K90 fine powder is added wherein, magnetic agitation gets evenly brown spinning liquid after 24 hours.After solution prepares, extract a certain amount of PVP spinning solution with syringe, be fixed on the electrostatic spinning apparatus, regulate various spinning parameters and carry out electricity and spin, the nanofiber that obtains is F 1Change Fe 3O 4Amount be that the nanofiber that 0.1g and 0.2g obtain is respectively F 2And F 3
Electricity is spun the nanofiber that obtains to be taken off from aluminium foil; Put into the there-necked flask of 250ml; Be that 80% ethanol water (PH=9.0) adds wherein and under 40 ℃ condition with preprepared ethanol volumetric concentration afterwards; Brute force stirs (100r/min) 24h, promptly gets the Fe of ferromagnetism different-grain diameter 3O 4/ SiO 2Nanoparticle.
Electro spinning nano fiber is characterized with SEM, and the result sees Fig. 1.With Fe 3O 4/ SiO 2Magnetic nano particle uses FESEM (TEM), XRD and VSM to characterize respectively, and the result sees Fig. 2, Fig. 4 and Fig. 5.Fibre diameter and Fe 3O 4/ SiO 2Relation between particle diameter is seen Fig. 3.
Embodiment 2
Press following step preparing spinning solution: with 0.025g Fe 3O 4, 0.2g CTAB and 0.8mL TEOS is dissolved separates in the Erlenmeyer flask that fills the 10mL isopropyl alcohol; Sonicated 20min afterwards; Then 0.9g PVP K90 fine powder is added wherein, magnetic agitation gets evenly brown spinning liquid after 24 hours.After solution prepares, extract a certain amount of PVP spinning solution, be fixed on the electrostatic spinning apparatus, regulate various spinning parameters and carry out electricity to spin the nanofiber that obtains be F with syringe 1Change Fe 3O 4Amount be that the nanofiber that 0.1g and 0.4g obtain is respectively F 2And F 3
When electricity spun, the syringe specification was 5mL, and the syringe needle internal diameter is about 1mm, and receiving screen adopts the reception of aluminium foil ground connection; The ejection flow velocity is 2-3.5mL/h, voltage 10-13kv, and the distance of syringe needle and receiving screen is 15-18cm.
Electricity is spun the nanofiber that obtains to be taken off from aluminium foil; Put into the there-necked flask of 250ml; Be that 70% ethanol water (PH=8.0) adds wherein and under 30 ℃ condition with preprepared ethanol volumetric concentration afterwards; Brute force stirs (300r/min) 24h, promptly gets the Fe of ferromagnetism different-grain diameter 3O 4/ SiO 2Nanoparticle.
Embodiment 3
Press following step preparing spinning solution: with 0.05g Fe 3O 4, 0.2g CTAB and 0.8mL TEOS is dissolved separates in the Erlenmeyer flask that fills the 10mL isopropyl alcohol; Sonicated 20min afterwards; Then 1.2g PVP K90 fine powder is added wherein, magnetic agitation gets evenly brown spinning liquid after 24 hours.After solution prepares, extract a certain amount of PVP spinning solution, be fixed on the electrostatic spinning apparatus, regulate various spinning parameters and carry out electricity to spin the nanofiber that obtains be F1 with syringe.Change Fe 3O 4Amount be that the nanofiber that 0.1g and 0.2g obtain is respectively F2 and F3.
When electricity spun, the syringe specification was 5mL, and the syringe needle internal diameter is about 1mm, and receiving screen adopts the reception of aluminium foil ground connection; The ejection flow velocity is 2-3.5mL/h, voltage 10-13kv, and the distance of syringe needle and receiving screen is 15-18cm.
Electricity is spun the nanofiber that obtains to be taken off from aluminium foil; Put into the there-necked flask of 250ml; Be that 80% ethanol water (PH=10.0) adds wherein and under 20 ℃ condition with preprepared ethanol volumetric concentration afterwards; Brute force stirs (300r/min) 24h, promptly gets the Fe of ferromagnetism different-grain diameter 3O 4/ SiO 2Nanoparticle.

Claims (10)

1. nucleocapsid Fe that particle diameter is controlled 3O 4/ SiO 2The preparation method of nanoparticle comprises:
(1) with Fe 3O 4, softex kw and ethyl orthosilicate be dissolved in the solvent, after the sonicated mixed solution; And then the adding polyvinylpyrrolidonepowder powder, stir, get brown spinning solution;
(2) adopt above-mentioned spinning solution to carry out electrostatic spinning, obtain nanofiber;
(3) above-mentioned nanofiber is placed ethanol water, under 20 ℃-40 ℃, stir, promptly get nucleocapsid Fe with speed 100-500r/min 3O 4/ SiO 2Nanoparticle.
2. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: the Fe described in the step (1) 3O 4, softex kw and ethyl orthosilicate amount ratio be 0.05-0.2g:0.1-0.2g:0.25-1.0mL.
3. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: the solvent described in the step (1) is an isopropyl alcohol.
4. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: the polyvinylpyrrolidone described in the step (1) is polyvinylpyrrolidone K90, and molecular weight is 360000.
5. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: the consumption and the Fe of the polyvinylpyrrolidone described in the step (1) 3O 4Mass ratio be 0.8-1.2:0.05-0.2.
6. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: Fe in the spinning solution described in the step (1) 3O 4Concentration be 0.002-0.008g/mL.
7. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: the syringe specification of being selected for use in the electrostatic spinning described in the step (2) is 5mL, and the syringe needle internal diameter is 1mm, and receiving screen adopts the reception of aluminium foil ground connection.
8. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: the technological parameter of the electrostatic spinning described in the step (2) is: the ejection flow velocity is 2-3.5mL/h, voltage 10-13kv, and the distance of syringe needle and receiving screen is 15-18cm.
9. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: the volume ratio 80-100:20-50 of ethanol and distilled water in the ethanol water described in the step (3); The pH value of described ethanol water is 8.0-10.0.
10. the nucleocapsid Fe that a kind of particle diameter according to claim 1 is controlled 3O 4/ SiO 2The preparation method of nanoparticle is characterized in that: the resulting nucleocapsid Fe of step (3) 3O 4/ SiO 2The saturation magnetization of nanoparticle is 30-50emu/g.
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ITTO20131037A1 (en) * 2013-12-18 2015-06-19 Fond Istituto Italiano Di Tecnologia PROCEDURE FOR ENCAPSING A LIQUID
CN105672014A (en) * 2016-03-01 2016-06-15 山东农业大学 Preparation method of super-hydrophobic magnetic nano-crystalline cellulose paper
CN107362775A (en) * 2017-07-17 2017-11-21 河北科技大学 A kind of core-shell structure magnetic fibre shape nano SiO 2 particle and its preparation method and application
CN109012568A (en) * 2018-07-06 2018-12-18 中南大学 A kind of nanofiber-based hud typed adsorbent material of magnetic silicon oxide and preparation method thereof
CN110042500A (en) * 2018-01-15 2019-07-23 哈尔滨工业大学 A kind of preparation method of ferroso-ferric oxide/silica composite fiber microwave absorbing material
CN113351239A (en) * 2020-03-05 2021-09-07 华东理工大学 Nickel-based pure silicon type molecular sieve catalyst and preparation method and application thereof

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CN102247803A (en) * 2011-05-04 2011-11-23 中国科学院化学研究所 Core-shell type magnetic mesoporous nano-microsphere as well as preparation method and application thereof
CN102623125A (en) * 2012-03-28 2012-08-01 东华大学 Preparation method for Fe3O4/SiO2 nanometer particle containing multiple magnetism cores

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KR20100123072A (en) * 2009-05-14 2010-11-24 전북대학교산학협력단 Core-shell typed cobalt/carbon composite nanofiber and method of manufacturing the same
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103011178A (en) * 2013-01-06 2013-04-03 东华大学 Preparation method of spherical SiO2 particles
ITTO20131037A1 (en) * 2013-12-18 2015-06-19 Fond Istituto Italiano Di Tecnologia PROCEDURE FOR ENCAPSING A LIQUID
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CN107362775A (en) * 2017-07-17 2017-11-21 河北科技大学 A kind of core-shell structure magnetic fibre shape nano SiO 2 particle and its preparation method and application
CN110042500A (en) * 2018-01-15 2019-07-23 哈尔滨工业大学 A kind of preparation method of ferroso-ferric oxide/silica composite fiber microwave absorbing material
CN109012568A (en) * 2018-07-06 2018-12-18 中南大学 A kind of nanofiber-based hud typed adsorbent material of magnetic silicon oxide and preparation method thereof
CN113351239A (en) * 2020-03-05 2021-09-07 华东理工大学 Nickel-based pure silicon type molecular sieve catalyst and preparation method and application thereof

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Application publication date: 20121128