CN101117241A - Ferrum oxidate nano magnetic material and method for preparing the same - Google Patents
Ferrum oxidate nano magnetic material and method for preparing the same Download PDFInfo
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- CN101117241A CN101117241A CNA200710043843XA CN200710043843A CN101117241A CN 101117241 A CN101117241 A CN 101117241A CN A200710043843X A CNA200710043843X A CN A200710043843XA CN 200710043843 A CN200710043843 A CN 200710043843A CN 101117241 A CN101117241 A CN 101117241A
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Abstract
The invention relates to a nanomagnetic material of iron oxide and the fabrication method, and belongs to the nano-material fabrication field; the invention adopts glycol as a solvent and a reducing agent, and adopts sodium dodecyl benzene sulfonate as a surfactant, and adopts dissoluble trivalent iron sodium and alkali as a raw material, a mixing process under a room temperature is conducted to make a homogeneous suspension; the mixed liquid is turned into a polytetrafluoroethene lining to conduct a microwave water thermal reaction, after the reaction is over, the product from the reaction is separated, washed and dried to make a precursor nano-powder which is calcined to make a ferroferric oxide nano-powder or gamma ferric oxide nano-powder; the nano-powder body has a hollow ball structure assembled by a nano-piece, the hollow ball dimension is two to four micron while the inner hollow dimension of the hollow ball is one to three micron; the invention is characterized in low raw material cost, easy process, easy operation, controllable profile and so forth; the specific surface area is high, the magnetic performance is favorable.
Description
Technical field
The present invention relates to oxidate nano magnetic material of a kind of iron and preparation method thereof, belong to field of nano material preparation.
Background technology
In recent years, the synthetic interest that has attracted more and more investigators as an important field of research of nano magnetic material.(D.B.Yu, X.Q.Sun, J.W.Zou, Z.R.Wang, F.Wang, K.Tang, J.Phys.Chem.B2006,110,21667; M.Arruebo, M.Gal á n, N.Navascu é s, C.T é llez, C.Marquina, M.R.Ibarra, J.Santamar í a, Chem.Mater.2006,18,1911.) because its good magnetic performance, chemical stability, biocompatibility and hypotoxicity, the research of nano magnetic material not only has been confined to the research of basic science, and expands to the especially research of targeted drug transportation of biomedicine field.(J.M.Nam, C.S.Thaxton, C.A.Mirkin, Science2003,301,1884; I.Willner, E.Katz, Angew.Chem.2003,115,4724; Angew.Chem.Int.Ed.2003,42,4576; M.Zhao, M.F.Kircher, L.Josephson, R.Weissleder, Bioconjugate Chem.2002,13,840; D.Hogemann, V.Ntziachristos, L.Josephson, R.Weissleder, Bioconjugate Chem.2002,13,116; F.Hu, L.Wei, Z.Zhou, Y.L.Ran, Z.Li, M.Y.Gao, Adv.Mater. 2006,18, and 2553; M.Br hler, R.Georgieva, N.Buske, A.M ü ller, S.M ü ller, J.Pinkernelle, U.Teichgr ber, A.Voigt, H.B umler, NanoLett.2006,6,2505; A.K.Gupta, M.Gupta.Biomaterials 2005,26,1565.) utilize externally-applied magnetic field can make the diseased region enrichment in vivo of nano magnetic target pharmaceutical carrier, reduce the medicine contact of healthy tissues, reduce toxic side effect, can effectively reduce amount of drug, improve the curative effect of medicine.And the nano magnetic material that is used for the target transportation is generally Z 250 and γ-ferric oxide.
Z 250 and γ-ferric oxide nano material good prospects for application has stimulated the fast development of its synthesis technique.In recent years, the investigator has been developed and multiple different synthetic method, as: coprecipitation method (S.H.Gee, Y.K.Hong, D.W.Erickso, M.H.Park, J.Appl.Phys.2003,93,7560.), microemulsion method (L.A.Harris, J.D.Goff, A.Y.Carmichael, J.S.Riffle, J.J.Harburn, T.G.S.Pierre, M.Saunders, Chem.Mater.2003,15,1367.), ultrasonic radiation method (V.G.Pol, M.Motiei, A.Gedanken, J.Calderon-Moreno, Y.Mastai, Chem.Mater.2003,15,1378.), hydrothermal method (Y.Sahoo, M.Cheon, S.Wang, H.Luo, E.P.Furlani, P.N.Prasad, J.Phys.Chem.B2004,108,3380.), organometallic compound thermal decomposition method (J.L.Lyon, D.A.Fleming, M.B.Stone, P.Schiffer, M.E.Williams, NanoLett.2004,4,719.) etc.The nano magnetic material of different-shape prepares.But, have high specific surface area and good magnetic performance, and the magneticsubstance with hollow ball that nanometer sheet is assembled into is not synthesized also.The present invention adopts single ferric ion source---and solubility trivalent iron salt and highly basic are raw material, prepare the nano magnetic material of Z 250 and γ-ferric oxide simultaneously, widened their application prospects in biomedicine field, catalytic field and magnetic resolution field.
Summary of the invention
Goal of the invention provides oxidate nano magnetic material of a kind of iron and preparation method thereof.
Concrete technology as shown in Figure 1.Concrete steps are:
1. the preparation of liquid-phase reaction system: with ethylene glycol as solvent and reductive agent, with the Sodium dodecylbenzene sulfonate is tensio-active agent, with solubility trivalent iron salt (comprising iron(ic) chloride, ferric sulfate, iron nitrate etc.) and highly basic (one or both of sodium hydroxide and potassium hydroxide) is that raw material is prepared reaction system, obtains homogeneous suspension by stirring.The concentration of described Sodium dodecylbenzene sulfonate is the 0.02-0.2 mol, and the concentration of solubility trivalent iron salt is the 0.02-0.2 mol, and alkaline concentration is the 0.1-1 mol.
2. homogeneous suspension is transferred to and carries out the microwave hydrothermal processing in the water heating kettle under 120-220 ℃, the microwave hydrothermal treatment time is 60-90 minute.Loading level is 1/4th to 1/2nd in the water heating kettle.Better effects if when water heating kettle has polytetrafluoroethyllining lining or directly is the tetrafluoroethylene material.
3. the product in the liquid-phase reaction system after microwave hydrothermal being handled separates, and separated products is washed and drying treatment, and drying temperature is 60-100 ℃, at air drying.
4. dried product is calcined in nitrogen, obtained the ferriferrous oxide nano powder.Calcining temperature is 200-450 ℃, and calcination time is no less than 1 hour.
5. dried product is calcined in air, obtained γ-ferric oxide nanometer powder.Calcining temperature is 200-450 ℃, and calcination time is no less than 1 hour.
The material component that preparation method provided by the invention obtains is respectively Z 250 and γ-ferric oxide, and they have the hollow ball structure that nanometer sheet is assembled into.Hollow ball is of a size of the 2-4 micron, the hollow 1-3 micron that is of a size of of hollow ball inside.
The preparation method of the oxidate nano magnetic material of iron provided by the invention and the material that obtains have the following advantages:
(1) utilizes the oxidate nano magnetic material of preparing two kinds of different iron with a kind of precursor first.
(2) ethylene glycol plays the effect (solvent) of complexing in precursor nanostructure synthetic, plays the effect of reductive agent simultaneously.This has simplified preparation process greatly, has reduced cost.
(3) raw material is cheap and easy to get, and is easy to operate, and preparation technology is simple, do not need cost and complex equipment, is easy to realize suitability for industrialized production.
(4) oxidate nano magnetic material of prepared iron has high specific surface area (Z 250 62m
2/ g, γ-ferric oxide 56m
2/ g) and good magnetic performance (with the Z 250 saturation magnetization rate after poly ethyldiol modified is 31.4emu/g, is 48.3emu/g with the γ after poly ethyldiol modified-ferric oxide susceptibility).
Description of drawings
Preparation technology's schema of the oxidate nano magnetic material of Fig. 1 iron
The X-ray powder diffraction spectrogram of Fig. 2 precursor
The electron scanning micrograph of the hollow ball that is assembled into by the precursor nanometer sheet that Fig. 3 obtained at 200 ℃ of microwave hydrothermals in 90 minutes: the hollow ball diameter is the 2-4 micron
The transmission electron microscope photo of the hollow ball that is assembled into by the precursor nanometer sheet that Fig. 4 obtained at 200 ℃ of microwave hydrothermals in 90 minutes
The electron scanning micrograph of Fig. 5 precursor hollow ball that calcining obtained in 1 hour in nitrogen under 300 ℃ is assembled into by ferroferric oxide nano-piece: the hollow ball diameter is the 2-4 micron
Fig. 6 precursor electron scanning micrograph by γ-hollow ball that the ferric oxide nanometer sheet is assembled into that calcining obtained in 1 hour in air under 300 ℃: the hollow ball diameter is the 2-4 micron
Embodiment
Further specify embodiment and effect with detail description embodiment.
Embodiment 1.
At room temperature, 0.541 gram iron chloride hexahydrate and 0.600 gram Sodium dodecylbenzene sulfonate are dissolved in 20 milliliters of ethylene glycol, the stirring at room dissolving obtains homodisperse solution.Restrain dissolution of sodium hydroxide in 10 milliliters of ethylene glycol with 0.160 in addition, the stirring at room dissolving obtains homodisperse solution.Mix above-mentioned two kinds of solution, stirring at room obtains homodisperse suspension.Get 20 milliliters of suspension and change (the liner capacity is 60 milliliters) in the polytetrafluoroethyllining lining over to, sealing.Liner is put into the microwave hydrothermal reaction unit, be incubated 90 minutes down at 200 ℃.After reaction system naturally cools to room temperature, take out product, use the centrifuging separated product, absolute ethanol washing 3 times of isolating product, 60 ℃ of air dryings obtain precursor.Precursor is put into tube furnace, and logical nitrogen atmosphere was calcined 1 hour down in 300 ℃, obtained the ferroferric oxide powder of black.Analysis revealed, product pattern are the hollow ball that nanometer sheet is assembled into, and median size is the 2-4 micron.
Embodiment 2.
At room temperature, 0.541 gram iron chloride hexahydrate and 0.600 gram Sodium dodecylbenzene sulfonate are dissolved in 20 milliliters of ethylene glycol, the stirring at room dissolving obtains homodisperse solution.Restrain dissolution of sodium hydroxide in 10 milliliters of ethylene glycol with 0.160 in addition, the stirring at room dissolving obtains homodisperse solution.Mix above-mentioned two kinds of solution, stirring at room obtains homodisperse suspension.Get 20 milliliters of suspension and change (the liner capacity is 60 milliliters) in the polytetrafluoroethyllining lining over to, sealing.Liner is put into the microwave hydrothermal reaction unit, be incubated 90 minutes down at 200 ℃.After reaction system naturally cools to room temperature, take out product, use the centrifuging separated product, absolute ethanol washing 3 times of isolating product, 60 ℃ of air dryings obtain precursor.Precursor is put into tube furnace, under 300 ℃, in air, calcined 1 hour, obtain the γ-ferric oxide powder of reddish-brown.Analysis revealed, product pattern are the hollow ball that nanometer sheet is assembled into, and median size is the 2-4 micron.
Claims (7)
1. the oxidate nano magnetic material of an iron is characterized in that component is a Z 250, has the hollow ball structure that nanometer sheet is assembled into, and hollow ball is of a size of the 2-4 micron, the hollow 1-3 micron that is of a size of of hollow ball inside.
2. the oxidate nano magnetic material of an iron is characterized in that component is γ-ferric oxide, has the hollow ball structure that nanometer sheet is assembled into, and hollow ball is of a size of the 2-4 micron, the hollow 1-3 micron that is of a size of of hollow ball inside.
3. the preparation method by the oxidate nano magnetic material of the described iron of claim 1 comprises that the preparation of reaction system, microwave hydrothermal are handled, separation, washing, drying and the calcination process of precursor, it is characterized in that comprising following step:
(1) with ethylene glycol as solvent and reductive agent, be tensio-active agent with the Sodium dodecylbenzene sulfonate, be raw material with solubility trivalent iron salt and highly basic, form homogeneous suspension under the room temperature; The concentration of described Sodium dodecylbenzene sulfonate is the 0.02-0.2 mol, and the concentration of solubility trivalent iron salt is the 0.02-0.2 mol, and alkaline concentration is the 0.1-1 mol;
(2) homogeneous suspension is transferred to carries out microwave hydrothermal in the water heating kettle and handle, the microwave hydrothermal treatment time is 60-90 minute, and loading level is 1/4th to 1/2nd in the water heating kettle.
(3) product in the liquid-phase reaction system after the microwave hydrothermal processing is separated, to the separated products absolute ethanol washing, and drying treatment;
(4) dried product is calcined in nitrogen or argon gas, calcining temperature is 200-450 ℃, and calcination time is no less than 1 hour.
4. the preparation method by the oxidate nano magnetic material of the described iron of claim 3 comprises that the preparation of reaction system, microwave hydrothermal are handled, separation, washing, drying and the calcination process of precursor, it is characterized in that comprising following step:
(1) with ethylene glycol as solvent and reductive agent, be tensio-active agent with the Sodium dodecylbenzene sulfonate, be raw material with solubility trivalent iron salt and highly basic, form homogeneous suspension under the room temperature; The concentration of described Sodium dodecylbenzene sulfonate is the 0.02-0.2 mol, and the concentration of solubility trivalent iron salt is the 0.02-0.2 mol, and alkaline concentration is the 0.1-1 mol;
(2) homogeneous suspension is transferred to carries out microwave hydrothermal in the water heating kettle and handle, the microwave hydrothermal treatment time is 60-90 minute, and loading level is 1/4th to 1/2nd in the water heating kettle.
(3) product in the liquid-phase reaction system after the microwave hydrothermal processing is separated, to the separated products absolute ethanol washing, and drying treatment;
(4) dried product is calcined in air, calcining temperature is 200-450 ℃, and calcination time is no less than 1 hour.
5. by claim 3 or 4 described a kind of preparation methods that prepare the oxidate nano magnetic material of iron, it is characterized in that used iron ion source is single solubility trivalent iron salt, comprises iron(ic) chloride, ferric sulfate, iron nitrate.
6. by claim 3 or 4 described a kind of methods that prepare the oxidate nano magnetic material of iron, it is characterized in that used highly basic is one or both of sodium hydroxide and potassium hydroxide.
7. by claim 1 or 2 described a kind of methods that prepare the oxidate nano magnetic material of iron, it is characterized in that described water heating kettle has polytetrafluoroethyllining lining or directly is the tetrafluoroethylene material.
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