CN1321898C - Prepn process of nanometer ferromagnetic oxide particle - Google Patents
Prepn process of nanometer ferromagnetic oxide particle Download PDFInfo
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- CN1321898C CN1321898C CNB2005101092162A CN200510109216A CN1321898C CN 1321898 C CN1321898 C CN 1321898C CN B2005101092162 A CNB2005101092162 A CN B2005101092162A CN 200510109216 A CN200510109216 A CN 200510109216A CN 1321898 C CN1321898 C CN 1321898C
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- oxide particle
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Abstract
The present invention discloses a method for preparing nanometer particles of ferromagnetic oxide, which comprises the following step: making a metallic ion solution react in a mixed system of alkali metal hydroxide, fatty acid and an organic polar solvent to obtain the nanometer particles of ferromagnetic oxide. The present invention forms a mixed solvent system by the fatty acid and the polar solvent. The method uses soluble metal salt and the alkali metal hydroxide as raw materials to prepare the nanometer particles of ferromagnetic oxide. The method of the present invention has the advantages of convenience, safety, low cost and wide applicability; simultaneously, the method for preparing nanometer particles of ferromagnetic oxide is suitable for synthesizing nanometer various kinds of particles of noble metal; the present invention overcomes the problems of high cost and environmental pollution because a large number of organic solvents is used in the existing synthetic route; the acquired nanometer particles of ferromagnetic oxide can be applied to the fields of biology, medicine, catalytic action, analysis, etc.
Description
Technical field
The present invention relates to a kind of method for preparing nanometer ferromagnetic oxide particle.
Background technology
Nanometer ferromagnetic oxide particle has in fields such as catalysis, medicine, analysis and biologies widely to be used.People such as Sun SH reported in hexadecanediol-oleic acid-oleylamine system, with iron (III) acetylacetonate (Fe (acac) on " American Chemical Society's meeting will " in 2004
3) pyrolysis at high temperature prepare the nanocrystalline method of ferromagnetic oxide (2004,126 the volume, the 273-279 page or leaf); Gao M.Y. etc. reported FeCl in 2005 on " German applied chemistry "
3Method in pyrroline liquid-phase system pyrolytic decomposition has been synthesized Fe
3O
4Nanocrystalline method (2005,44 volumes, 123-126 page or leaf); People such as Li Yadong reported to be that solvent, polyvinyl alcohol are the method for protective material synthesizing magnetic wustite micron ball with ethylene glycol in 2005 on " German applied chemistry ", size is in 200 nanometers～1 micron (2005,44 volumes, 2782-2785 page or leaf).Among the above-mentioned preparation method, used system is organic solvent system, has not only increased production cost greatly, also will inevitably bring problem of environmental pollution; And the brilliant product of institute synthetic magnetic Nano all is suspended in organic solution with the colloidal particle form, needs to adopt a large amount of alcohol organic solvent that it is separated, and gives further to amplify and brought difficulty.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing nanometer ferromagnetic oxide particle.
The method for preparing nanometer ferromagnetic oxide particle provided by the present invention is that metal ion solution is reacted in the mixed system of alkali metal hydroxide, lipid acid and organic polar solvent, obtains described nanometer ferromagnetic oxide particle.
Wherein, the step of above-mentioned reaction is: earlier solid alkali metal oxyhydroxide is joined in the mixed solvent of lipid acid and organic polar solvent, add metal ion solution after the mixing again 20-300 ℃ of reaction down, obtain described nanometer ferromagnetic oxide particle.
In preparation process, the volume ratio of lipid acid and organic polar solvent is 1: 0.5-10; The concentration of metal ion solution is 0.01-0.5mol/L, and the volume ratio of metal ion solution and mixed solvent is 1: 0.5-5; The mol ratio of alkali metal hydroxide and metal ion is 1-10: 1.In used metal ion chosen from Fe, manganese, cobalt, magnesium and the zine ion etc. one or more can pass through these metal soluble salt, and waiting as nitrate, hydrochloride, vitriol or acetate provides.Lipid acid is oleic acid, stearic acid or capric acid etc.Organic polar solvent is ethanol, acetone, ethylene glycol or glycerol etc.
The present invention constitutes mixed solvent system with lipid acid and polar solvent, is raw material with soluble metallic salt and alkali metal hydroxide, prepares nanometer ferromagnetic oxide particle.The inventive method is easy, safety, cost is low, suitability is wide, be applicable to the synthetic of multiple noble metal nano particles simultaneously, overcome and adopted cost and the problem of environmental pollution that a large amount of organic solvent brought in the existing synthetic route, the nanometer ferromagnetic oxide particle that is obtained can be applied to fields such as biology, medicine, catalysis and analysis.
Description of drawings
Fig. 1 is the prepared Z 250 X-ray powder diffraction figure of embodiment 1.
Fig. 2 is that embodiment 1 prepared Z 250 TEM Electronic Speculum detects figure.
Fig. 3 is the prepared iron cobalt oxygen X-ray powder diffraction figure of embodiment 3.
Fig. 4 is that embodiment 3 prepared iron cobalt oxygen TEM Electronic Speculum detect figure.
Fig. 5 is the prepared ferrimanganic oxygen X-ray powder diffraction figure of embodiment 5.
Fig. 6 is that embodiment 5 prepared ferrimanganic oxygen TEM Electronic Speculum detect figure.
Fig. 7 is the prepared iron magnesia X-ray powder diffraction figure of embodiment 7.
Fig. 8 is that embodiment 7 prepared iron magnesia TEM Electronic Speculum detect figure.
Embodiment
Embodiment 1,
Taking by weighing 1.0gNaOH adds in 10ml oleic acid, the 8ml ethanol mixed solvent, in, fully behind the about 30mins of reaction, take by weighing 1g analytical pure sulfuric acid ferrous ammonium and be dissolved in the 18mL water, and the ferric ion solutions that is made into is added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 140 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as Z 250 through X-ray powder diffraction as shown in Figure 1; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 2 its pattern is the dispersed nano particle, and particle diameter is between 4-5nm.
Embodiment 2:
Taking by weighing 0.5gKOH adding 20ml is dissolved with in the stearic ethylene glycol solvent of 5g, fully behind the about 30mins of reaction, taking by weighing 2g analytical pure sulfuric acid ferrous ammonium is dissolved in the 20mL water, and with in the ferric ion solutions adding mixed solvent that is made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 240 ℃ of reaction 24h, the gained precipitation obtains black powder after centrifugation, washing, drying.Product is accredited as Z 250 through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 10-20nm.
Embodiment 3:
Taking by weighing 0.8gNaOH adds in 5ml oleic acid, the 20ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 0.8g analytical pure sulfuric acid ferrous ammonium is dissolved in the 7mL water, take by weighing 0.3g analytical pure cobalt chloride and be dissolved in the 8mL water, iron ion, the cobalt ion solution that is made into is added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 120 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as iron cobalt oxygen through X-ray powder diffraction as shown in Figure 3; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 4 its pattern is the dispersed nano particle, and particle diameter is between 5-6nm.
Embodiment 4:
Taking by weighing 2gKOH adds in the mixed solvent of 10ml oleic acid, 20ml acetone, fully behind the about 30mins of reaction, taking by weighing 0.5g analytical pure sulfuric acid ferrous ammonium is dissolved in the 5mL water, take by weighing 0.2g analytical pure Xiao Suangu and be dissolved in the 5mL water, iron ion, the cobalt ion solution that is made into is added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 180 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as iron cobalt oxygen through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 20-30nm.
Embodiment 5:
Taking by weighing 1gNaOH adds in 6ml oleic acid, the 18ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 1.0g analytical pure sulfuric acid ferrous ammonium is dissolved in the 8mL water, take by weighing 0.2g analytical pure sulfuric acid manganese and be dissolved in the 8mL water, iron ion, the mn ion solution that is made into is added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 170 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as ferrimanganic oxygen through X-ray powder diffraction as shown in Figure 5; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 6 its pattern is the dispersed nano particle, and particle diameter is between 2-3nm.
Embodiment 6:
Taking by weighing 3gKOH adds in 5ml capric acid, the 20ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 0.6g analytical pure sulfuric acid ferrous ammonium is dissolved in the 7mL water, take by weighing 0.1g analytical pure sulfuric acid manganese and be dissolved in the 8mL water, iron ion, the mn ion solution that is made into is added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 20 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as ferrimanganic oxygen through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 20-30nm.
Embodiment 7:
Taking by weighing 0.5gNaOH adds in 8ml oleic acid, the 15ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 1.0g analytical pure sulfuric acid ferrous ammonium is dissolved in the 9mL water, take by weighing 0.4g analytical pure magnesium nitrate and be dissolved in the 8mL water, iron ion, the magnesium ion solution that is made into added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 200 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as the iron magnesia through X-ray powder diffraction as shown in Figure 7; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 8 its pattern is the dispersed nano particle, and particle diameter is between 2-4nm.
Embodiment 8:
Taking by weighing 0.5gNaOH adds in 8ml oleic acid, the 15ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 0.4g analytical pure sulfuric acid ferrous ammonium is dissolved in the 9mL water, take by weighing 0.1g analytical pure magnesium nitrate and be dissolved in the 8mL water, iron ion, the magnesium ion solution that is made into added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 110 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as the iron magnesia through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 20-40nm.
Embodiment 9:
Taking by weighing 1gNaOH adds in 10ml oleic acid, the 10ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 1.0g analytical pure sulfuric acid ferrous ammonium is dissolved in the 10mL water, take by weighing 0.5g analytical pure zinc chloride and be dissolved in the 10mL water, iron ion, the zine ion solution that is made into is added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 170 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as iron zinc oxygen through X-ray powder diffraction as shown in Figure 9; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 10 its pattern is the dispersed nano particle, and particle diameter is between 3-4nm.
Embodiment 10:
Taking by weighing 0.4gKOH adds in the mixed solvent of 6ml oleic acid, 20ml glycerol, fully behind the about 30mins of reaction, taking by weighing 0.8g analytical pure sulfuric acid ferrous ammonium is dissolved in the 7mL water, take by weighing 0.4g analytical pure zinc nitrate and be dissolved in the 7mL water, iron ion, the zine ion solution that is made into is added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 180 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as iron zinc oxygen through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 50-60nm.
Claims (3)
1, a kind of method for preparing nanometer ferromagnetic oxide particle, be to be that the metal ion solution of 0.01-0.5mol/L reacts in the mixed system of alkali metal hydroxide, lipid acid and organic polar solvent, obtain described nanometer ferromagnetic oxide particle concentration; The volume ratio of described lipid acid and organic polar solvent is 1: 0.5-10; The volume ratio of the mixed solvent that described metal ion solution and lipid acid and organic polar solvent are formed is 1: 0.5-5; The mol ratio of described alkali metal hydroxide and described metal ion is 1-10: 1; Described lipid acid is oleic acid, stearic acid or capric acid; Described organic polar solvent is ethanol, acetone, ethylene glycol or glycerol.
2, method according to claim 1, it is characterized in that: the step of described reaction is: earlier solid alkali metal oxyhydroxide is joined in the mixed solvent of lipid acid and organic polar solvent composition, add metal ion solution after the mixing again 20-300 ℃ of reaction down, obtain described nanometer ferromagnetic oxide particle.
3, according to claim 1 or 2 or 3 described methods, it is characterized in that: one or more in described metal ion chosen from Fe, manganese, cobalt, magnesium and the zine ion.
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| CNB2005101092162A CN1321898C (en) | 2005-10-19 | 2005-10-19 | Prepn process of nanometer ferromagnetic oxide particle |
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| CNB2005101092162A CN1321898C (en) | 2005-10-19 | 2005-10-19 | Prepn process of nanometer ferromagnetic oxide particle |
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| CN1321898C true CN1321898C (en) | 2007-06-20 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323046A (en) * | 2001-06-07 | 2001-11-21 | 东南大学 | Composite nanometer magnetic titania material with Mn-Zn ferrite and its prepn |
| CN1486958A (en) * | 2003-04-01 | 2004-04-07 | 上海大学 | Prepn of doped magnetic ferrite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323046A (en) * | 2001-06-07 | 2001-11-21 | 东南大学 | Composite nanometer magnetic titania material with Mn-Zn ferrite and its prepn |
| CN1486958A (en) * | 2003-04-01 | 2004-04-07 | 上海大学 | Prepn of doped magnetic ferrite material |
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