CN101993115B - Preparation method of ferroferric oxide magnetic nanoparticles - Google Patents
Preparation method of ferroferric oxide magnetic nanoparticles Download PDFInfo
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- CN101993115B CN101993115B CN2009101946062A CN200910194606A CN101993115B CN 101993115 B CN101993115 B CN 101993115B CN 2009101946062 A CN2009101946062 A CN 2009101946062A CN 200910194606 A CN200910194606 A CN 200910194606A CN 101993115 B CN101993115 B CN 101993115B
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Abstract
The invention belongs to the field of nanometer materials, in particular relates to a preparation method of ferroferric oxide magnetic nanoparticles. The preparation method comprises the following steps of: dissolving ferric trichloride or ferric nitrate in an alcoholic solvent to form a uniformly dispersed alcoholic solution; then adding epoxy propane or epoxy chloropropane to form a sol, and forming a gel after standing; and aging, washing, drying and annealing the prepared gel to prepare the ferroferric oxide magnetic nanoparticles. The preparation method has the advantages of simple and available raw materials required for preparation, low cost, narrow particle size and good roundness of the prepared nanoparticles, simple process flow and higher purity of products, and continuous production mode is easy to establish.
Description
Technical field
The invention belongs to field of nanometer material technology, be specifically related to a kind of preparation method of ferroferric oxide magnetic nanoparticle.
Background technology
In recent years, because the extensive prospect of magnetic nano-particle in practical application, about the preparation method and the performance of magnetic nanometer receives great concern.At biomedical sector, particle diameter because of having nano-meter characteristic and superparamagnetism concurrently, has wide application prospect in fields such as cell marking, albumen sepn, medicine controlled releasing, NMR contrast agent and tumour magnetic thermotherapies less than the magnetic nanoparticle of 20nm; Aspect magnetic recording material, magnetic nano-particle is expected to replace the micron order magnetic, is used for the high density magnetic recording material; Aspect new forms of energy, the magnetohydrodynamic generator of processing with magnetic nano-particle will become the strong additional of conventional energy resources.
The nanometer Fe 3 O 4 magnetic powder is a kind of novel fine chemical product; Because it has general unrivaled property of fast body material and purposes at aspects such as light, electricity, medicine, magneticmedium; So can be widely used in fields such as national defence, Surface Engineering, environmental engineering, chemical industry, electronic material and semiconductor material, have very application prospects.As in industrial aspect, magnetic nano-particle can be used for the preparation of high density magnetic recording magnetic head; At biological technical field, the various preparations of processing with magnetic nano-particle have been widely used in the separation of biological sample, nuclear magnetic resonance, fields such as immunodetection and drug targeting release.Yet it as the lubricating system additive, especially as the aqueous lubricating system, all is significant in theory research and industrial application.But because therefore the high reactivity of ferriferrous oxide nano-particle and huge surface-area when it forms the heterogeneous system of high dispersing in water, exist huge interface between particle and the medium.Simultaneously, ferriferrous oxide nano-particle has high surface energy, can cause the thermodynamic phase of dispersion system, and ferriferrous oxide nano-particle can attract each other, and formation is reunited and precipitated.Therefore, improving the dispersion stabilization of ferriferrous oxide nano-particle, is the problem that this nano material must solve in application process.Simultaneously, the nanometer Fe 3 O 4 magnetic powder in actual application, except require particle diameter regular shape, particle diameter enough little, also need require the centralized particle diameter of particle, be easy to form monodispersed ion.
In the prior art, the preparation method of ferroferric oxide magnetic nanoparticle has chemical coprecipitation, high-temperature decomposition, mini-emulsion process and sol-gel method etc.Wherein chemical coprecipitation is to study the most a kind of method, and it is through to containing Fe
3+And Fe
2+Add alkaline matter (like NaOH solution or ammoniacal liquor etc.) in the solution and prepare Fe as precipitation agent
3O
4The magnetic nanoparticle its essence is Fe
3+And Fe
2+Ion hydrolytic precipitation under alkaline condition makes Fe
3O
4The magnetic nanoparticle.Though this method is simple to operate and expend cheaply, the magnetic nanoparticle out-of-shape of preparing, is easy to reunite the size distribution broad, be difficult to form monodispersed particle, and difficult technique is with control.Therefore, this area is badly in need of the preparation method of the ferroferric oxide magnetic nanoparticle that a kind of technology is simple, with low cost, product performance are stable at present.
Summary of the invention
The objective of the invention is to deficiency, a kind of preparation method of ferroferric oxide magnetic nanoparticle is provided to prior art.
The present invention realizes above-mentioned technical problem through following technical scheme:
A kind of preparation method of ferroferric oxide magnetic nanoparticle comprises the steps:
1) iron trichloride or iron nitrate are dissolved in the finely dispersed alcoholic solution of formation in the alcoholic solvent;
2) add propylene oxide or epoxy chloropropane formation colloidal sol in the alcoholic solution that in step 1), makes, leave standstill the back and form gel;
3) with step 2) in the gel that makes after ageing, clean and dry;
4) cleaning and dried gel in the step 3) being carried out anneal can make.
Preferable, the alcoholic solvent in the said step 1) is selected from: methyl alcohol, ethanol, pinakon, and perhaps wherein any two kinds mixture, perhaps the mixture of methyl alcohol, ethanol and pinakon further is preferably ethanol.
Preferable, in the alcoholic solution in the said step 1), the concentration of iron ion is 0.8～1.5mol/L, further is preferably 0.9～1.2mol/L.
Preferable, in the said step 1), also need in alcoholic solution, add zero(ppm) water, and the add-on of zero(ppm) water is 0～4ml, further be preferably 2～3ml.The adding of zero(ppm) water can promote the hydrolysis of iron ion in alcoholic solvent, makes hydrolysis rate accelerate.
Preferable, the dispersing method in the said step 1) is a ultra-sonic dispersion.
Preferable, said step 2) in, the mol ratio of propylene oxide or epoxy chloropropane and iron ion is 6～20: 1, more preferably 6～14: 1.
Term " mol ratio of propylene oxide or epoxy chloropropane and iron ion " is meant: the mol ratio of propylene oxide and iron ion, perhaps, the mol ratio of epoxy chloropropane and iron ion.
Preferable, said step 2) time of repose in is 1～40 minute, more preferably 1～20 minute.
Preferable, the digestion time in the said step 3) is 1～24h, 2～4h more preferably, and the ageing temperature is a room temperature.
Preferable, the concrete steps of the cleaning in the said step 3) are: add absolute ethyl alcohol and carry out ultrasonic cleaning, the time of each ultrasonic cleaning is 15～60 minutes, and washing times is 2～5 times.
Preferable, the exsiccant concrete steps in the said step 3) are: seasoning is 15～45 days in the air ambient, more preferably 20～25 days; Perhaps be positioned over the loft drier drying, be 4～48h its time of drying, 6～12h more preferably, and drying temperature is 30～80 ℃, more preferably 35～45 ℃.
Preferable, the concrete steps of the anneal of said step 4) are: in air atmosphere or vacuum, under 250～450 ℃ temperature condition, anneal; Annealing time is 0.5～2h, is preferably 0.5-1h.
Preferred, the concrete steps of the anneal of said step 4) are: in air atmosphere, be 250～300 ℃ in annealing temperature and anneal; Perhaps in a vacuum, being 300～350 ℃ in annealing temperature anneals.
Through detection, the nano particle diameter narrow range of the ferroferric oxide nano granules that preparation method of the present invention makes, roundness is good.Simultaneously, the present invention adopts sol-gel method to prepare ferroferric oxide magnetic nanoparticle, and in this preparation process, the adding of propylene oxide helps forming fast gel, can prevent that like this particulate is grown up in the gel formation process.Anneal is this preparing method's a committed step, and the anneal that (comprises the control of annealing atmosphere and annealing temperature) under the conditions suitable can promote the formation of nanoparticle, and removes contained organism and moisture, obtains the pure nano Z 250.Preparing method of the present invention has following advantage: 1) the required medicine of preparation and starting material are simple and easy to, and are with low cost; 2) adopt sol-gel method to prepare, nano material, its technical process is simple, sets up the mode of production of continous way easily; 3) preparation method of the present invention can make highly purified nano ferriferrous oxide.
Description of drawings
The XRD figure of the ferroferric oxide magnetic nanoparticle that makes among Fig. 1 embodiment 1.
The TEM figure of the ferroferric oxide magnetic nanoparticle that makes among Fig. 2 embodiment 1.
Embodiment
Further specify the present invention below in conjunction with embodiment, but the present invention is not limited to these concrete embodiments; Any change or improvement on basis of the present invention all belongs to protection scope of the present invention.
Embodiment 1:
1, the preparation of ferroferric oxide magnetic nanoparticle:
1) take by weighing iron trichloride, it is dissolved in the ethanol of 11ml, make the concentration of its iron ion reach 0.9mol/L, add 2ml zero(ppm) water, ultra-sonic dispersion is even;
2) in the above-mentioned solution that makes, add propylene oxide and form colloidal sol, wherein the molar ratio of iron ion and propylene oxide is 1: 9; Above-mentioned colloidal sol was left standstill 3 minutes, promptly form gel;
3) with behind the prepared gel ageing 4h, add absolute ethyl alcohol, carry out ultrasonic cleaning, washing times is 3 times, each washing time is 20 minutes;
4) gel after will washing was positioned in the air ambient seasoning 15 days;
5) sample after the drying is carried out anneal, its annealing atmosphere is an air, and annealing temperature is 250 ℃, and annealing time is 2h, finally can obtain the nano ferriferrous oxide powder.
2, the character of ferroferric oxide magnetic nanoparticle detects:
1) with X-ray diffraction analysis (XRD); Referring to Fig. 1, can confirm that by the XRD figure of Fig. 1 prepared black powder is the Z 250 of magnetite structure, and product purity is very high; Adopt Jade5.0 software to calculate through Scherrer (Scherrer) formula, the median size of nanoparticle is 10.5nm;
2) utilize the H-800 of Hitachi transmission electron microscope (TEM) to observe, concrete TEM figure is referring to Fig. 2, by knowing among Fig. 2 that prepared ferriferrous oxide particles is spherical; Roundness is high; Complete in crystal formation, its particle size range is: 9～12nm and conforms to Scherrer (Scherrer) formula institute result calculated.
Embodiment two:
1, the preparation of ferroferric oxide magnetic nanoparticle:
1) take by weighing iron trichloride, it is dissolved in the ethanol of 9ml, make the concentration of its iron ion reach 1.1mol/L, add 1ml zero(ppm) water, ultra-sonic dispersion is even;
2) in the above-mentioned solution that makes, add propylene oxide and form colloidal sol, wherein the molar ratio of iron ion and propylene oxide is 1: 12; Above-mentioned colloidal sol was left standstill 2 minutes, promptly form gel;
3) with behind the prepared gel ageing 4h, add absolute ethyl alcohol, carry out ultrasonic cleaning, washing times is 3 times, each washing time is 15 minutes;
4) gel after will washing is positioned over the loft drier drying, and be 24h its time of drying, and drying temperature is 40 ℃;
5) sample after the drying is carried out anneal, its annealing atmosphere is a vacuum, and annealing temperature is 300 ℃, finally can obtain the nano ferriferrous oxide powder.
2, the character of ferroferric oxide magnetic nanoparticle detects:
1) with X-ray diffraction analysis (XRD), can confirm that prepared black powder is the Z 250 of magnetite structure, and product purity is very high, to calculate through Scherrer (Scherrer) formula, the median size of nanoparticle is 8.6nm;
2) utilize the H-800 of Hitachi transmission electron microscope (TEM) to observe, can see prepared ferriferrous oxide particles for spherical, roundness is high, complete in crystal formation, and its particle size range is: 8～11nm and conforms to Scherrer (Scherrer) formula institute result calculated.
Embodiment three:
1, the preparation of ferroferric oxide magnetic nanoparticle:
1) take by weighing iron trichloride, it is dissolved in the 1L ethanol, make the concentration of its iron ion reach 0.8mol/L, add 4ml zero(ppm) water, ultra-sonic dispersion is even;
2) in the above-mentioned solution that makes, add epoxy chloropropane and form colloidal sol, wherein iron ion and epoxy chloropropane molar ratio are 1: 6; Above-mentioned colloidal sol was left standstill 40 minutes, promptly form gel;
3) with behind the prepared gel ageing 24h, add absolute ethyl alcohol, carry out ultrasonic cleaning, washing times is 5 times, each washing time is 60 minutes;
4) gel after will washing was positioned in the air ambient seasoning 45 days;
5) sample after the drying is carried out anneal, its annealing atmosphere is an air atmosphere, and annealing temperature is 300 ℃, finally can obtain the nano ferriferrous oxide powder.
2, the character of ferroferric oxide magnetic nanoparticle detects:
1) with X-ray diffraction analysis (XRD), can confirm that prepared black powder is the Z 250 of magnetite structure, and product purity is very high, to calculate through Scherrer (Scherrer) formula, the median size of nanoparticle is 13.1nm;
2) utilize the H-800 of Hitachi transmission electron microscope (TEM) to observe, can see prepared ferriferrous oxide particles for spherical, roundness is high, complete in crystal formation, and its particle size range is: 10～14nm and conforms to Scherrer (Scherrer) formula institute result calculated.
Embodiment four:
1, the preparation of ferroferric oxide magnetic nanoparticle:
1) take by weighing the 1.5mol iron trichloride, it is dissolved in the mixture of 1L methyl alcohol, ethanol and pinakon, make the concentration of its iron ion reach 1.5mol/L, ultra-sonic dispersion is even;
2) in the above-mentioned solution that makes, add the 30mol epoxy chloropropane and form colloidal sol, wherein iron ion and epoxy chloropropane molar ratio are 1: 20; Above-mentioned colloidal sol was left standstill 1 minute, promptly form gel;
3) with behind the prepared gel ageing 1h, add absolute ethyl alcohol, carry out ultrasonic cleaning, washing times is 2 times, each washing time is 15 minutes;
4) gel after will washing was positioned in the air ambient seasoning 15 days;
5) sample after the drying is carried out anneal, its annealing atmosphere is a vacuum atmosphere, and annealing temperature is 350 ℃, finally can obtain the nano ferriferrous oxide powder.
2, the character of ferroferric oxide magnetic nanoparticle detects:
1) with X-ray diffraction analysis (XRD), can confirm that prepared black powder is the Z 250 of magnetite structure, and product purity is very high, to calculate through Scherrer (Scherrer) formula, the median size of nanoparticle is 11nm;
2) utilize the H-800 of Hitachi transmission electron microscope (TEM) to observe, can see prepared ferriferrous oxide particles for spherical, roundness is high, complete in crystal formation, and its particle size range is: 9.5～12nm and conforms to Scherrer (Scherrer) formula institute result calculated.
Embodiment five:
1, the preparation of ferroferric oxide magnetic nanoparticle:
1) take by weighing the 1.0mol iron nitrate, it is dissolved in 1L pinakon and the alcoholic acid mixture, make the concentration of its iron ion reach 1.0mol/L, ultra-sonic dispersion is even;
2) in the above-mentioned solution that makes, add the 10mol epoxy chloropropane and form colloidal sol, wherein iron ion and epoxy chloropropane molar ratio are 1: 10; Above-mentioned colloidal sol was left standstill 25 minutes, promptly form gel;
3) with behind the prepared gel ageing 15h, add absolute ethyl alcohol, carry out ultrasonic cleaning, washing times is 3 times, each washing time is 20 minutes;
4) gel after will washing is positioned over the loft drier drying, and be 48h its time of drying, and drying temperature is 80 ℃;
5) sample after the drying is carried out anneal, its annealing atmosphere is a vacuum, and annealing temperature is 450 ℃, finally can obtain the nano ferriferrous oxide powder.
2, the character of ferroferric oxide magnetic nanoparticle detects:
1) with X-ray diffraction analysis (XRD), can confirm that prepared black powder is the Z 250 of magnetite structure, and product purity is very high, to calculate through Scherrer (Scherrer) formula, the median size of nanoparticle is 13.4nm;
2) utilize the H-800 of Hitachi transmission electron microscope (TEM) to observe, can see prepared ferriferrous oxide particles for spherical, roundness is high, complete in crystal formation, and its particle size range is: 11～15nm and conforms to Scherrer (Scherrer) formula institute result calculated.
Embodiment six:
1, the preparation of ferroferric oxide magnetic nanoparticle:
1) take by weighing the 1.2mol iron nitrate, it is dissolved in 1L methyl alcohol and the alcoholic acid mixture, make the concentration of its iron ion reach 1.2mol/L, ultra-sonic dispersion is even;
2) in the above-mentioned solution that makes, add the 16.8mol epoxy chloropropane and form colloidal sol, wherein iron ion and epoxy chloropropane molar ratio are 1: 14; Above-mentioned colloidal sol was left standstill 22 minutes, promptly form gel;
3) with behind the prepared gel ageing 4h, add absolute ethyl alcohol, carry out ultrasonic cleaning, washing times is 2 times, each washing time is 20 minutes;
4) gel after will washing is positioned over the loft drier drying, and be 4h its time of drying, and drying temperature is 30 ℃;
5) sample after the drying is carried out anneal, its annealing atmosphere is a vacuum, and annealing temperature is 400 ℃, finally can obtain the nano ferriferrous oxide powder.
2, the character of ferroferric oxide magnetic nanoparticle detects:
1) with X-ray diffraction analysis (XRD), can confirm that prepared black powder is the Z 250 of magnetite structure, and product purity is very high, to calculate through Scherrer (Scherrer) formula, the median size of nanoparticle is 12.6nm;
2) utilize the H-800 of Hitachi transmission electron microscope (TEM) to observe, can see prepared ferriferrous oxide particles for spherical, roundness is high, complete in crystal formation, and its particle size range is: 11～14nm and conforms to Scherrer (Scherrer) formula institute result calculated.
Claims (4)
1. the preparation method of a ferroferric oxide magnetic nanoparticle comprises the steps:
1) iron trichloride or iron nitrate are dissolved in the finely dispersed alcoholic solution of formation in the alcoholic solvent, said alcoholic solvent is selected from: methyl alcohol, ethanol, perhaps methyl alcohol, alcoholic acid mixture, the perhaps mixture of methyl alcohol, ethanol and pinakon; In the said alcoholic solution, the concentration of iron ion is 0.8～1.5mol/L;
2) add propylene oxide or epoxy chloropropane formation colloidal sol in the alcoholic solution that in step 1), makes, leave standstill the back and form gel, the mol ratio of said propylene oxide or epoxy chloropropane and iron ion is 6～20: 1;
3) with step 2) in the gel that makes after ageing, clean and dry;
4) cleaning and dried gel in the step 3) are carried out anneal and can make ferroferric oxide magnetic nanoparticle; The concrete steps of said anneal are: in air atmosphere or vacuum, under 250～450 ℃ temperature condition, anneal.
2. the preparation method of the ferroferric oxide magnetic nanoparticle described in claim 1 is characterized in that, in the said step 1), also need in alcoholic solution, add zero(ppm) water, and the add-on of zero(ppm) water is 0～4mL.
3. the preparation method of the ferroferric oxide magnetic nanoparticle described in claim 1; It is characterized in that; The concrete steps of the cleaning in the said step 3) are: add absolute ethyl alcohol and carry out ultrasonic cleaning, each washing time is 15～60 minutes, and washing times is 2～5 times.
4. the preparation method of the ferroferric oxide magnetic nanoparticle described in claim 1 is characterized in that, the exsiccant concrete steps in the said step 3) are: seasoning is 15～45 days in the air ambient; Perhaps be positioned over the loft drier drying, be 4～48h its time of drying, and drying temperature is 30～80 ℃.
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| CN102660220A (en) * | 2012-04-16 | 2012-09-12 | 天津大学 | Preparation method of graphene supported ferriferrous oxide nanocomposite |
| CN103723773B (en) * | 2012-10-16 | 2016-06-29 | 国家纳米科学中心 | A kind of hydrosol of ferroferric oxide nano granules and its preparation method and application |
| CN104817117A (en) * | 2015-04-30 | 2015-08-05 | 江苏大学 | Preparation method of adjustable particle size aerogel-skeleton ferroferric oxide |
| CN105905949B (en) * | 2016-04-13 | 2017-12-15 | 江苏中兴药业有限公司 | A kind of magnetic Fe3O4/Fe2O3The preparation method of composite nanorod |
| CN108311107B (en) * | 2018-01-19 | 2020-11-27 | 武汉工程大学 | Epichlorohydrin modified Fe3O4Magnetic nano material and preparation and application thereof |
| CN110102264B (en) * | 2019-06-04 | 2021-03-02 | 太原理工大学 | Preparation of ultra-high magnetic responsiveness nanocluster microspheres and wastewater treatment method |
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| CN101113022A (en) * | 2007-07-06 | 2008-01-30 | 哈尔滨工业大学 | Chitose aquagel evoked original position synthesis of super-paramagnetism nano ferriferrous oxide particles |
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| CN101113022A (en) * | 2007-07-06 | 2008-01-30 | 哈尔滨工业大学 | Chitose aquagel evoked original position synthesis of super-paramagnetism nano ferriferrous oxide particles |
Non-Patent Citations (3)
| Title |
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| JP昭61-281023A 1986.12.11 |
| Wei Wu et al..Magnetic Iron Oxide Nanoparticles: Synthesis and Surface Functionalization Strategies.《Nanoscale Res Lett》.2008,第3卷397-415. * |
| 李成魁 等.磁性纳米四氧化三铁颗粒的化学制备及应用进展.《上海金属》.2009,第31卷(第4期),54-58. * |
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