CN1195305C - High specific saturated magnetizing strengh Fe3O4 micro particles and its preparing method - Google Patents

High specific saturated magnetizing strengh Fe3O4 micro particles and its preparing method Download PDF

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CN1195305C
CN1195305C CNB031252605A CN03125260A CN1195305C CN 1195305 C CN1195305 C CN 1195305C CN B031252605 A CNB031252605 A CN B031252605A CN 03125260 A CN03125260 A CN 03125260A CN 1195305 C CN1195305 C CN 1195305C
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fe3o4
particulate
saturation magnetization
specific saturation
magnetic
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CN1474417A (en
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程海斌
袁润章
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Wuhan University of Science and Engineering WUSE
Wuhan University of Technology WUT
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Abstract

The present invention discloses a Fe3O4 microparticle with high specific saturation magnetization and a preparation method thereof. The specific saturation magnetization of the Fe3O4 microparticle with high specific saturation magnetization reaches more than 80 emu/g. The preparation method of the Fe3O4 microparticle with high specific saturation magnetization comprises: organic surface active agents are added into the solution of nano Fe3O4 microparticles, which is obtained in the traditional technique for preparing Fe3O4 microparticles, the solution of nano Fe3O4 microparticles and the organic surface active agents are together added into a nano-processing machine, microparticles are further pulverized and have a force chemical reaction with organic macromolecular compounds under the action of large mechanical force of the nano-processing machine, the surface modification for inorganic particles is realized, the tendency to form bridge bonds among the nano Fe3O4 microparticles is prevented, and the obtain nano Fe3O4 microparticles have small particle size, uniform particle distribution, good dispersivity, high stability and high specific saturation magnetization. The present invention solves the technical problem that the specific saturation magnetization of Fe3O4 microparticles is low and unstable; the present invention is especially suitable for preparing magnetized liquids, magnetized microspheres, magnetized drugs, etc.

Description

A kind of Fe 3O 4Particulate and preparation method thereof
Technical field
The present invention relates to Fe 3O 4Particulate and preparation method thereof, particularly a kind of high specific saturation magnetization Fe 3O 4Particulate and preparation method thereof.
Background technology
Fe 3O 4Just be widely used in preparing magnetic liquid, magnetic micro-beads, magnetic and medicated etc. as magnetic particle.Such as the nanometer Fe with high magnetic 3O 4The magnetic liquid that particle is made, be applied to Dynamic Sealing sealing, loudspeaker, damping device, Mineral separation, precise finiss etc., magnetic microsphere is applied to magnetic chemiluminescence immune assay, cell separation, purify protein, separate nucleic acid, target administration etc., has huge using value.Fe 3O 4The important indicator that particulate is used for above field is specific saturation magnetization, and it is more high more good to require.But the Fe that reports at present 3O 4The specific saturation magnetization of particulate is all lower.Particularly because due to the quantum size effect of nano particle, the specific saturation magnetization of particle reduces with diameter and reduces.So, nanometer Fe 3O 4The specific saturation magnetization of particulate is generally all very low.Comprise the nanometer Fe with the preparation of the methods such as sonar chemical method, coprecipitation, oxidizing process 3O 4Particulate, its specific saturation magnetization below 80emu/g, generally are below 60emu/g all, and what have only has several emu/g, and because of the different nanometer Fe that make of preparation condition control 3O 4The specific saturation magnetization of particulate is widely different.Work as nanometer Fe 3O 4Particulate is applied to magnetic liquid, magnetic micro-beads, when magnetic and medicated, requires particle diameter enough little on the one hand, and is more thin more good, requires on the other hand the specific saturation magnetization of magnetic grain more high more good.As when magnetic and medicated, particle is big then may to be caused in the human body inner accumulated, particularly may in blood vessel, gather and artery-clogging, cause side effect and can't use, if the low targeted therapy function that then is difficult to reach the target effect and loses targeted drug of specific saturation magnetization.So, necessarily require particle diameter little, the specific saturation magnetization height.This is just so that the nanometer Fe of conventional method preparation 3O 4Particulate is being applied to prepare magnetic liquid, magnetic micro-beads, is being restricted when magnetic and medicated etc.
Summary of the invention
The present invention seeks in order to overcome Fe 3O 4The limitation that the specific saturation magnetization of particulate is low and defective provide a kind of high specific saturation magnetization Fe 3O 4Particulate and preparation method thereof, this Fe 3O 4Particulate has high specific saturation magnetization, particle diameter is little, particle diameter is evenly distributed, good dispersion, stable high, can be used for preparation
The technical scheme that the present invention takes is: prepare Fe in tradition 3O 4On the basis of particulate technology, introduce nano-dispersed and surface modification technology, tradition is prepared Fe 3O 4The nanometer Fe that obtains in the particulate technology 3O 4Particulate solution, add surfactant, particularly adopted a kind of " power chemistry " method, being about to them together joins in the machine of a kind of being called " nanometer machine " (Beijing Jin Haina Science and Technology Ltd.), (operation principle of this machine is to apply huge mechanical force in moment to reactant, make inorganic particulate moment be broken into sub-micron or nanometer particle, make organic high molecular compound in solvent, form the nanoscale microemulsion, the inorganic particles of synkaingenesis and organic high molecular compound microemulsion force lower fierce collision and force-chemical reaction take place in huge mechanical force, form chemical bonding), under the huge mechanical force of " nanometer machine ", particulate further pulverized and with organic high molecular compound generation force-chemical reaction, inorganic particulate reaches finishing, has stoped nanometer Fe 3O 4Form the strong tendency of bridging oxygen between the particulate, the nanometer Fe that obtains 3O 4Diameter of particle is little and be evenly distributed good dispersion, stability height, specific saturation magnetization height.Be adapted to especially prepare magnetic liquid, magnetic micro-beads, magnetic and medicated etc.
Fe of the present invention 3O 4Particulate, its specific saturation magnetization 〉=80emu/g, average grain diameter is 5～1000nm, and average grain diameter is preferably 5～500nm, and average grain diameter is 10～30nm preferably.
Fe of the present invention 3O 4The preparation method of particulate, its preparation process is as follows:
1st, the air that is equipped with in the reactor of stirring, filling with inert gas, constant pressure funnel, vacuum extractor is replaced with filling with inert gas argon gas or nitrogen;
2nd, be respectively to take by weighing trivalent iron salt and divalent iron salt at 2: 1 in molar ratio, drop in the ready reactor of step 1, add the deoxidation dissolved in purified water of 20～50 times of weight, stir into homogeneous solution;
3rd, 4～8 times by the molysite total mole number take by weighing NaOH, become the NaOH aqueous solution of 1～6mol/L with the deoxidation dissolved in purified water, add constant pressure funnel, are stirring and N 2Or splash in the reactor under the Ar gas shiled, make the pH value of mixed molysite solution progressively be elevated to 8～10, obtain dark solution;
4th, the dark solution that obtains to step 3 adds the aqueous solution of surfactant, surfactant can be a kind of in anionic surfactant, cationic surface active agent, the nonionic surface active agent, also can be their mixture, stir 1～2h then;
5th, the product that obtains in the step 4 is joined in the nanometer machine, regulate earlier mechanical force 600～2000kgf/cm 2Or be divided into for two steps, be earlier 600～1000kgf/cm 2Pulverize and finishing, regulating then mechanical force is 1000～2000kgf/cm 2, further pulverize and finishing, obtain all good black magnetic liquid of dispersed and stability;
6th, the product that step 5 is obtained is removed the individual coarse particle with the speed centrifugation of 2000～8000rpm, obtains the black magnetic nanometer Fe of uniform stable dispersion 3O 4Magnetic solution;
7th, the black magnetic particulate that step 6 is obtained respectively washs 2 times with ethanol, deoxidation pure water, acetone respectively, adopts magnet to separate in the washing process, removes moisture and the solvent on magnetic grain surface;
8th, the black magnetic particulate drying 5～8h that step 7 is obtained, 60～100 ℃ of drying 6～8h, 120 ℃ of drying 5～8h namely obtain high-purity saturation magnetization Fe 3O 4Particulate.
Above-mentioned trivalent iron salt is FeCl 36H 2O or (NH 4) Fe (SO 4) 2
Above-mentioned divalent iron salt is FeCl 24H 2O or FeSO 47H 2O.
Above-mentioned surfactant is preferentially selected in oleic acid, enuatrol, DBSA, lauryl sodium sulfate, the alkyl polyoxyethylene ether any.
Characteristics of the present invention are:
(1) utilized " force-chemical reaction principle ", power energy and chemical energy are combined, after huge mechanical force can be pulverized particle, this nascent nano particle has huge surface energy, high activity is arranged, surfactant also can be dispersed into molecule solution by huge power simultaneously, has equally huge activity, to nanometer Fe 3O 4Particulate produces strong chemical bonding, and with the increase of putting forth effort, this bonding will be towards intermolecular bonding, and particle further diminishes, the further attenuation of outer field organic film.
(2) Fe that makes of this law 3O 4Particulate has high specific saturation magnetization, can reach more than the 80emu/g.
(3) preparation technology is simple, but the scale preparation has high specific saturation magnetization Fe 3O 4Particulate.
Method of the present invention not only can be applicable to nanometer Fe 3O 4The preparation of particulate also can be used for the preparation of other ferrite and nano-metal-oxide.The Fe that makes 3O 4Particulate has high specific saturation magnetization, and for the preparation of magnetic liquid, magnetic micro-beads, when magnetic and medicated etc., consumption is few, and magnetic responsiveness is good.
After generally having narrated the present invention, by can further understanding the present invention with reference to some specific embodiment provided by the invention, described embodiment only is in order to describe the present invention in detail, certainly to be not intended to limit the present invention's meaning.Fully can improve and change the present invention according to above-mentioned explanation, still within interest field of the present invention.
Description of drawings
Fig. 1 is Fe of the present invention 3O 4Nanometer Fe with conventional method 3O 4Specific saturation magnetization.
Embodiment
Embodiment 1: produce as follows Fe 3O 4Particulate
1,1000ml four necks of stirring, filling with inert gas, constant pressure funnel, vacuum extractor will be housed
1, the air in the flask will be housed at the bottom of the 1000ml four neck gardens of stirring, filling with inert gas, constant pressure funnel, vacuum extractor replaces with nitrogen;
2, take by weighing 3.2g FeCl respectively 36H 2O (AR) and 1.7g FeSO 47H 2O (AR) drops in the ready reactor of step 1, adds the deoxidation dissolved in purified water of 50 times of weight, stirs into homogeneous solution;
3, take by weighing 4g NaOH (AR), with the NaOH aqueous solution of deoxidation pure water 400ml dissolving into about 3mol/L, add in the constant pressure funnel, stirring and N 2Splash in the reactor under the gas protection, obtain dark solution after dripping off;
4, in the dark solution that step 3 obtains, add the aqueous solution that contains 0.5g oleic acid, stir 1～2h;
5, the product that obtains in the step 4 is joined in the nanometer machine, setting earlier mechanical force is 1200kgf/cm 2, carry out force-chemical reaction, and circulate 3 times, then mechanical force is set at 1500kgf/cm 2, carry out force-chemical reaction, and circulate 3 times, obtain all good black magnetic liquid of dispersed and stability;
6, the product that step 5 is obtained supercentrifuge (GL21R high speed freezing centrifuge, Zhizheng Centrifugal Machines Co., ltd., Shanghai, together lower) with the speed centrifugation 30min of 6000rpm, remove the black magnetic nanometer Fe that the individual coarse particle obtains uniform stable dispersion 3O 4Magnetic solution;
7, the black magnetic particulate that step 6 is obtained respectively washs 2 times with ethanol, deoxidation pure water, acetone respectively, adopts magnet to separate in the washing process, removes moisture and the solvent on magnetic grain surface;
8, the black magnetic particulate that step 7 is obtained places vacuum drying chamber in 60 ℃ of drying 5～8h, 80 ℃ of drying 6～8h, and 120 ℃ of drying 5～8h namely obtain nanometer Fe 3O 4Particulate, measuring its specific area with (U.S. Gemini 2360V5.00) BET specific surface area measuring instrument is 63.1m 2/ g, average grain diameter is 18.3nm, produces the 3257-35 magnetometer with Japan, presses the HG/T2347.2-92 standard, measuring specific saturation magnetization at 25 ℃ is 115emu/g, sees Fig. 1.
Embodiment 2: produce as follows Fe 3O 4Particulate
1, the air in the flask will be housed at the bottom of the 1000ml four neck gardens of stirring, filling with inert gas, constant pressure funnel, vacuum extractor replaces with argon gas;
2, take by weighing 3.2g FeCl respectively 36H 2O (AR) and 1.2g FeCl 24H 2O (AR) drops in the ready reactor of step 1, adds the deoxidation dissolved in purified water of 50 times of weight, stirs into homogeneous solution;
3, take by weighing 5gNaOH (AR),, add constant pressure funnel, under stirring and Ar gas shiled, splash in the reactor, obtain dark solution after dripping off with the NaOH aqueous solution of deoxidation pure water 400ml dissolving into about 3mol/L;
4, in the dark solution that step 3 obtains, add the aqueous solution that contains the 0.6g enuatrol, stir 1～2h;
5, the product that obtains in the step 4 is joined in the nanometer machine, setting earlier mechanical force is 1300kgf/cm 2, carry out force-chemical reaction, and circulate 3 times, then mechanical force is set at 1500kgf/cm 2, carry out force-chemical reaction, and circulate 2 times, obtain all good black magnetic liquid of dispersed and stability;
6, the product supercentrifuge that step 5 is obtained with the speed centrifugation 30min of 6000rpm, is removed the black magnetic nanometer Fe that the individual coarse particle obtains uniform stable dispersion 3O 4Magnetic solution;
7, the black magnetic particulate that step 6 is obtained respectively washs 2 times with ethanol, deoxidation pure water, acetone respectively, adopts magnet to separate in the washing process, removes moisture and the solvent on magnetic grain surface;
8, the black magnetic particulate that step 7 is obtained places vacuum drying chamber in 60 ℃ of drying 5～8h, 80 ℃ of drying 6～8h, and 120 ℃ of drying 5～8h namely obtain nanometer Fe 3O 4Particulate, recording its specific area with the identical method of embodiment 1 and condition is 61.5m 2/ g, average grain diameter is 18.8nm, specific saturation magnetization is 103.4emu/g, sees Fig. 1.
Embodiment 3: produce as follows Fe 3O 4Particulate
1, the air in the flask will be housed at the bottom of the 1000ml four neck gardens of stirring, filling with inert gas, constant pressure funnel, vacuum extractor replaces with nitrogen;
2, take by weighing 4.0g NaOH (AR), drop in the ready reactor of step 1, add the deoxidation dissolved in purified water NaOH of 40 times of weight, stir into homogeneous solution;
3, take by weighing 3.2g FeCl respectively 36H 2O (AR) and 1.7g FeSO 47H 2O (AR), 1000ml is dissolved into the aqueous solution with the deoxidation pure water, adds constant pressure funnel, is stirring and N 2Splash in the reactor under the gas shiled, obtain dark solution after dripping off;
4, in the dark solution that step 3 obtains, add the aqueous solution that contains the 0.7g neopelex, stir 1～2h;
5, the product that obtains in the step 4 is joined in the nanometer machine, setting earlier mechanical force is 1300kgf/cm 2, carry out force-chemical reaction, and circulate 2, then mechanical force is set at 1400kgf/cm 2, carry out force-chemical reaction, and circulate 2, obtain all good black magnetic liquid of dispersed and stability;
6, the product supercentrifuge that step 5 is obtained with the speed centrifugation 30min of 6000rpm, is removed the black magnetic nanometer Fe that the individual coarse particle obtains uniform stable dispersion 3O 4Magnetic solution;
7, the black magnetic particulate that step 6 is obtained respectively washs 2 times with ethanol, deoxidation pure water, acetone respectively, adopts magnet to separate in the washing process, removes moisture and the solvent on magnetic grain surface;
8, the black magnetic particulate that step 7 is obtained places vacuum drying chamber in 60 ℃ of drying 5～8h, 80 ℃ of drying 6～8h, and 120 ℃ of drying 5～8h namely obtain nanometer Fe 3O 4Particulate, recording its specific area with the identical method of embodiment 1 and condition is 60.1m 2/ g, average grain diameter is 19.3nm, specific saturation magnetization is 92.3emu/g, sees Fig. 1.
Embodiment 4 produces Fe as follows 3O 4Particulate
1, the air in the flask will be housed at the bottom of the 1000ml four neck gardens of stirring, filling with inert gas, constant pressure funnel, vacuum extractor replaces with nitrogen;
2, take by weighing 4.0g NaOH (AR), drop in the ready reactor of step 1, add the deoxidation dissolved in purified water NaOH of 30 times of weight, stir into homogeneous solution;
3, take by weighing 3.2g FeCl respectively 36H 2O (AR) and 1.2g FeCl 24H 2O (AR), 1000ml is dissolved into the aqueous solution with the deoxidation pure water, adds constant pressure funnel, is stirring and N 2Splash in the reactor under the gas shiled, obtain dark solution after dripping off;
4, in the dark solution that step 3 obtains, add the aqueous solution that contains the 0.7g neopelex, stir 1～2h;
5, the product that obtains in the step 4 is joined in the nanometer machine, setting earlier mechanical force is 1300kgf/cm 2, carry out force-chemical reaction, and circulate 2, then mechanical force is set at 1400kgf/cm 2, carry out force-chemical reaction, and circulate 2, obtain all good black magnetic liquid of dispersed and stability;
6, the product high speed centrifugation that step 5 is obtained with the speed centrifugation 30min of 6000rpm, is removed the black magnetic nanometer Fe that the individual coarse particle obtains uniform stable dispersion 3O 4Magnetic solution;
7, the black magnetic particulate that step 6 is obtained respectively washs 2 times with ethanol, deoxidation pure water, acetone respectively, adopts magnet to separate in the washing process, removes moisture and the solvent on magnetic grain surface;
8, the black magnetic particulate that step 7 is obtained places vacuum drying chamber in 60 ℃ of drying 5～8h, 80 ℃ of drying 6～8h, and 120 ℃ of drying 5～8h namely obtain nanometer Fe 3O 4Particulate, recording its specific area with the identical method of embodiment 1 and condition is 59.8m 2/ g, average grain diameter is 19.3nm, specific saturation magnetization is 91.1emu/g, sees Fig. 1.
Embodiment 5 produces Fe as follows 3O 4Particulate
1, the air in the flask will be housed at the bottom of the 1000ml four neck gardens of stirring, filling with inert gas, constant pressure funnel, vacuum extractor replaces with nitrogen;
2, take by weighing 3.2g FeCl respectively 36H 2O (AR) and 1.7g FeSO 47H 2O (AR) drops in the ready reactor of step 1, adds 800ml deoxidation dissolved in purified water, stirs into homogeneous solution;
3, take by weighing 5g NaOH (AR), with the NaOH aqueous solution of deoxidation pure water 400ml dissolving into about 3mol/L, add in the constant pressure funnel, stirring and N 2Splash in the reactor under the gas protection, obtain dark solution after dripping off;
4, in the dark solution that step 3 obtains, add the aqueous solution that contains 0.5g dodecyl APEO, stir 1～2h;
5, the product that obtains in the step 4 is joined in the nanometer machine, setting earlier mechanical force is 1300kgf/cm 2, carry out force-chemical reaction, and circulate 5 times, obtain all good black magnetic liquid of dispersed and stability;
6, the product high speed centrifugation that step 5 is obtained with the speed centrifugation 30min of 6000rpm, is removed the black magnetic nanometer Fe that the individual coarse particle obtains uniform stable dispersion 3O 4Magnetic solution;
7, the black magnetic particulate that step 6 is obtained respectively washs 2 times with ethanol, deoxidation pure water, acetone respectively, adopts magnet to separate in the washing process, removes moisture and the solvent on magnetic grain surface;
8, the black magnetic particulate that step 7 is obtained places vacuum drying chamber in 60 ℃ of drying 5～8h, 80 ℃ of drying 6～8h, and 120 ℃ of drying 5～8h namely obtain nanometer Fe 3O 4Particulate, recording its specific area with the identical method of embodiment 1 and condition is 57.7m 2/ g, average grain diameter is 20.0nm, specific saturation magnetization is 89.4emu/g, sees Fig. 1.
Embodiment 6 (comparative example)
Prepare nanometer Fe by traditional coprecipitation 3O 4Particulate the steps include:
1, the air in the flask will be housed at the bottom of the 1000ml four neck gardens of stirring, filling with inert gas, constant pressure funnel, vacuum extractor replaces with nitrogen;
2, take by weighing 3.2gFeCl respectively 36H 2O (AR) and 1.7g (6mmol) FeSO 47H 2O (AR) drops in the ready reactor of step 1, adds 1000ml deoxidation dissolved in purified water, stirs into homogeneous solution;
3, take by weighing 6gNaOH (AR),, add constant pressure funnel with the NaOH aqueous solution of deoxidation pure water 400ml dissolving into about 3mol/L, under agitation, N 2Splash in the reactor under the gas shiled, obtain dark solution after dripping off;
4, the product high speed centrifugation that step 3 is obtained with the speed centrifugation 30min of 6000rpm, is removed corase particles (greatly increasing with the relatively more obvious corase particles of embodiment 1-5), obtains the black magnetic nanometer Fe 3O 4Magnetic solution;
5, the black magnetic particulate that step 4 is obtained respectively washs 2 times with ethanol, deoxidation pure water, acetone respectively, adopts magnet to separate in the washing process, removes moisture and the solvent on magnetic grain surface;
6, the black magnetic particulate that step 5 is obtained places vacuum drying chamber in 60 ℃ of drying 5～8h, 80 ℃ of drying 6～8h, and 120 ℃ of drying 5～8h namely obtain nanometer Fe 3O 4Particulate; Recording its specific area with the identical method of embodiment 1 and condition is 39.9m 2/ g, average grain diameter is 29.0nm, specific saturation magnetization is 45.6emu/g, sees Fig. 1.
Can see the nanometer Fe that makes with method of the present invention from above-mentioned example 3O 4Particulate, the height that its specific saturation magnetization all makes than conventional method.

Claims (5)

1, a kind of Fe 3O 4Particulate is characterized in that 80emu/g＜specific saturation magnetization≤115emu/g, and average grain diameter is 5～30nm.
2, the described Fe of claim 1 3O 4The preparation method of particulate is characterized in that preparation process is as follows:
1st, the air that will be equipped with in the reactor of stirring, filling with inert gas, constant pressure funnel, vacuum extractor is replaced with filling with inert gas argon gas or nitrogen;
2nd, be respectively to take by weighing trivalent iron salt and divalent iron salt at 2: 1 in molar ratio, drop in the ready reactor of step 1, add the deoxidation dissolved in purified water of 20～50 times of weight, stir into homogeneous solution;
3rd, 4～8 times by the molysite total mole number take by weighing NaOH, become the NaOH aqueous solution of 1～6mol/L with the deoxidation dissolved in purified water, add constant pressure funnel, are stirring and N 2Or splash in the reactor under the Ar gas shiled, make the pH value of mixed molysite solution progressively be elevated to 8～10, after obtain dark solution;
4th, the dark solution that obtains to step 3 adds the aqueous solution of surfactant, surfactant can be a kind of in anionic surfactant, cationic surface active agent, the nonionic surface active agent, also can be their mixture, stir 1～2h then;
5th, the product that obtains in the step 4 is joined in the nanometer machine, regulate mechanical force 600～2000kgf/cm 2Or be divided into for two steps, be earlier 600～1000kgf/cm 2Pulverize and finishing, regulating mechanical force then is 1000～2000kgf/cm 2, further pulverize and finishing, obtain black magnetic liquid dispersed and that stability is all good;
6th, the product that step 5 is obtained is removed the individual coarse particle with the speed centrifugation of 2000～8000rpm, obtains the black magnetic nanometer Fe of uniform stable dispersion 3O 4Magnetic solution;
7th, the black magnetic particulate that step 6 is obtained respectively washs 2 times with ethanol, deoxidation pure water, acetone respectively, adopts magnet to separate in the washing process, removes moisture and the solvent on magnetic grain surface;
8th, the black magnetic particulate substep that step 7 is obtained namely obtains high specific saturation magnetization Fe in 60 ℃ of drying 5～8h, 60～100 ℃ of drying 6～8h, 120 ℃ of drying 5～8h 3O 4Particulate.
3, method as claimed in claim 2 is characterized in that described trivalent iron salt is FeCl 36H 2O or (NH 4) Fe (SO 4) 2
4, method as claimed in claim 2 is characterized in that described divalent iron salt is FeCl 24H 2O or FeSO 47H 2O.
5, method as claimed in claim 2, it is characterized in that described surfactant be in oleic acid, enuatrol, DBSA, lauryl sodium sulfate, the alkyl polyoxyethylene ether any.
CNB031252605A 2003-08-13 2003-08-13 High specific saturated magnetizing strengh Fe3O4 micro particles and its preparing method Expired - Fee Related CN1195305C (en)

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CN1640819B (en) * 2004-09-01 2011-08-31 盛蓉生 Hydrophilic magnetic nano micro particle and its dispersion liquid preparing technique
CN100395852C (en) * 2004-11-12 2008-06-18 清华大学 Method for synthesizing series single-dispersed ferrite nanometer magnetic beads
CN1298791C (en) * 2005-07-19 2007-02-07 吉林大学 Superparamagnetic Fe3O4 nanometer particle with synthetic polymer modification from one-step method
CN100355661C (en) * 2005-12-01 2007-12-19 上海交通大学 Method for preparing polar solvent soluble nano ferriferrous oxide granule
CN100487831C (en) * 2006-10-23 2009-05-13 中国科学院过程工程研究所 Method for making magnetic nano particle based on solution co-deposition
CN101024518B (en) * 2007-01-30 2010-07-21 河北工业大学 Method for preparing Fe3O4 powder with ordered nano array structure
CN102249346B (en) * 2011-06-08 2013-03-20 哈尔滨工程大学 Preparation method for flower-like nanometer superstructure of ferroferric oxide
CN110801536B (en) * 2018-07-18 2021-01-01 中南大学 Organic-coated magnetic nanoparticle composite bone scaffold and preparation method thereof
CN109065319A (en) * 2018-09-12 2018-12-21 自贡兆强密封制品实业有限公司 A kind of superelevation saturation magnetization Fe3O4The preparation method of nano particle and its magnetic fluid
CN112164574A (en) * 2020-09-18 2021-01-01 天津大学 Preparation method of sodium dodecyl sulfate modified magnetic nanoparticles

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