CN101318709A - Method for preparing nano-gamma-Fe2O3 hollow magnetic microsphere - Google Patents
Method for preparing nano-gamma-Fe2O3 hollow magnetic microsphere Download PDFInfo
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- CN101318709A CN101318709A CNA2008100394915A CN200810039491A CN101318709A CN 101318709 A CN101318709 A CN 101318709A CN A2008100394915 A CNA2008100394915 A CN A2008100394915A CN 200810039491 A CN200810039491 A CN 200810039491A CN 101318709 A CN101318709 A CN 101318709A
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Abstract
The invention discloses a method for preparing gamma-Fe2O3 nanometer hollow magnetic microspheres, which comprises the following steps that: a certain quantity of sodium dodecylbenzenesulfonate (DBS) is added into 100ml of water, then a certain quantity of FeCl3.6H2O and Fe2(SO4)3 are added into the mixed liquid and stirred for 20 to 60 minutes, then urea is added into the mixed liquid, the mixed liquid is refluxed for 2 to 5 hours at a temperature of between 95 and 105 DEG C, and a precipitate is centrifugated, washed for a plurality of times, and dried at a temperature of 100 DEG C after alcohol being washed to produce an alpha-FeOOH precursor. The precursor is subject to heat treatment for 0.5 to 3 hours under an air atmosphere of between 250 and 400 DEG C, then the obtained product is subject to heat treatment for 1 to 3 hours under an H2 atmosphere of between 300 and 450 DEG C, finally the temperature is slowly decreased to between 150 and 250 DEG C, the atmosphere is changed from H2 to O2, and a final product is prepared after 1 to 3 hours of heat treatment. The product prepared by the method has high purity, definite compositions and crystal forms, and homogeneous hollow spherical structures.
Description
Technical field
The present invention relates to prepare the method for nano particle, especially prepare γ-Fe
2O
3The method of nano-hollow magnetic microsphere.
Background technology
Recently the preparation that has the nano material of special construction or pattern becomes the focus in investigation of materials field.As a kind of special nanostructure, the hollow ball shape nano material, owing to have the character of low density, high-ratio surface, and its hollow parts can hold a large amount of guest molecules or large-sized object, can produce some peculiar character, thereby enjoy people's attention based on microcosmic " encapsulation ", " parcel " effect.γ-Fe
2O
3It is a kind of application functional materials very widely, owing to have good magnetic, catalysis and air-sensitive performance and absorption and the shielding effect good to ultraviolet ray, it is used as magnetic recording material, magnetic liquid, electromagnetic wave absorbent material, gas sensor, catalyzer, nonlinear optical material, all has a good application prospect in fields such as electronics, petrochemical complex, environmental protection and biological medicine engineerings.γ-Fe
2O
3Preparation also be the focus that people study.The preparation method has comprised liquid-phase precipitation method, electrochemical process, template, hydrothermal method, laser vapor phase method, pyrolysis method, solid phase method etc.But up to the present, that people's report is γ-Fe mostly
2O
3The preparation of nano particle is about the γ-Fe of other pattern
2O
3Preparation less relatively.And some preparation method exists complicated operation, process to be difficult to control, quality product is difficult to weak points such as assurance.Therefore, explore a kind of method simple to operate, that process is easy to control and prepare γ-Fe with special appearance
2O
3Nanostructure becomes investigator's target.
Summary of the invention
The objective of the invention is to propose a kind of preparation γ-Fe
2O
3The method of nano-hollow magnetic microsphere.
Method of the present invention comprises the steps:
(1) a certain amount of Sodium dodecylbenzene sulfonate (DBS) is joined in the 100ml water, after adding a certain amount of iron trichloride and ferric sulfate stirring 30min then, add urea, with mixed solution backflow 2～5h under 100 ℃, and precipitate centrifugal, repeatedly the washing, alcohol wash the back 100 ℃ of oven dry, obtain the alpha-feooh presoma;
(2) with presoma thermal treatment 0.5～3h under 250～400 ℃ of air atmospheres;
(3) then with the product that obtains at 300～450 ℃ of H
2Thermal treatment 1～3h under the atmosphere slowly cools to 150～250 ℃ at last, with atmosphere by H
2Change O into
2, thermal treatment 1～3h had both obtained final product.
In the said mixed solution, the mol ratio of iron trichloride and ferric sulfate is 1.6～2.5, and the molar weight of urea is 15～20 times of molysite molar weight, content 0.002～0.006g/ml of DBS in the aqueous solution.
The product that adopts above-mentioned steps to obtain, by transmission electron microscope and scanning electron microscopic observation, the pattern of product is that the diameter of ball is about 200～300nm by integrated nano-hollow sphere structured of nanometer stub autohemagglutination, the crystalline phase of product consists of γ-Fe
2O
3(JCPDS No.39-1346).
The present invention adopts solution method to synthesize the alpha-feooh presoma, has prepared γ-Fe by the thermal treatment under the different condition then
2O
3Nano-hollow sphere structured, this method technology is simple, raw material is cheap, products therefrom purity height, component and crystal formation are determined and it is good nano-hollow sphere structured to have.
Description of drawings:
Fig. 1 is the x-ray diffraction pattern of embodiment 1 products therefrom.
Embodiment
Embodiment 1
Take by weighing 0.30g DBS and add in the 100ml deionized water, fully stir and add 0.27g iron trichloride and 0.20g ferric sulfate behind the 30min and stir and add 1.5g urea after for some time and continue to stir.Move into subsequently in the 250ml three hole bottles at 100 ℃ of backflow 3h.The precipitation that obtains is put into baking oven behind centrifugal, water Shen, pure Shen, 100 ℃ of oven dry down;
Above-mentioned powder is put into 300 ℃ of thermal treatment 2h in the retort furnace, puts into quartz tube furnace at 350 ℃ of H
2Thermal treatment 2h under the atmosphere slowly drops to 200 ℃ then at O
2Thermal treatment 2h under the atmosphere can obtain final product.The hollow ball structure that product is formed for the nanometer stub, crystallinity is good.The crystalline phase of product is formed as shown in Figure 1.
Take by weighing 0.50g DBS and add in the 100ml deionized water, fully stir and add 0.27g iron trichloride and 0.25g ferric sulfate behind the 30min and stir and add 1.8g urea after for some time and continue to stir.Move into subsequently in the 250ml three hole bottles at 100 ℃ of backflow 5h.The precipitation that obtains is put into baking oven after centrifugal, washing, alcohol are washed, 100 ℃ of oven dry down;
Above-mentioned powder is put into 300 ℃ of thermal treatment 2h in the retort furnace, puts into quartz tube furnace at 350 ℃ of H
2Thermal treatment 2h under the atmosphere slowly drops to 200 ℃ then at O
2Thermal treatment 3h under the atmosphere can obtain final product.The hollow ball structure that product is formed for the nanometer stub, crystallinity is good.
Embodiment 3
Take by weighing 0.40g DBS and add in the 100ml deionized water, fully stir and add 0.27g iron trichloride and 0.18g ferric sulfate behind the 30min and stir and add 1.40g urea after for some time and continue to stir.Move into subsequently in the 250ml three hole bottles at 100 ℃ of backflow 2h.The precipitation that obtains is put into baking oven after centrifugal, washing, alcohol are washed, 100 ℃ of oven dry down;
Above-mentioned powder is put into 350 ℃ of thermal treatment 1h in the retort furnace, puts into quartz tube furnace at 300 ℃ of H
2Thermal treatment 3h under the atmosphere slowly drops to 180 ℃ then at O
2Thermal treatment 3h under the atmosphere can obtain final product.The hollow ball structure that product is formed for the nanometer stub, crystallinity is good.
Embodiment 4
Take by weighing 0.60g DBS and add in the 100ml deionized water, fully stir and add 0.23g iron trichloride and 0.20g ferric sulfate behind the 30min and stir and add 1.6g urea after for some time and continue to stir.Move into subsequently in the 250ml three hole bottles at 100 ℃ of backflow 5h.The precipitation that obtains is put into baking oven after centrifugal, washing, alcohol are washed, 100 ℃ of oven dry down;
Above-mentioned powder is put into 400 ℃ of thermal treatment 1h in the retort furnace, puts into quartz tube furnace at 400 ℃ of H
2Thermal treatment 1.5h under the atmosphere slowly drops to 250 ℃ then at O
2Thermal treatment 2h under the atmosphere can obtain final product.The hollow ball structure that product is formed for the nanometer stub, crystallinity is good.
Claims (2)
1, a kind of preparation γ-Fe
2O
3The method of nano-hollow magnetic microsphere is characterized in that, comprises the steps:
(1) a certain amount of Sodium dodecylbenzene sulfonate is joined in the 100ml water, after adding a certain amount of iron trichloride and ferric sulfate stirring 20～60min then, add urea, with mixed solution backflow 2～5h under 95～105 ℃, and precipitate centrifugal, repeatedly washing, alcohol are washed back oven dry, obtain the alpha-feooh presoma;
Wherein, the mol ratio of iron trichloride and ferric sulfate is 1.6～2.5, and the molar weight of urea is 15～20 times of molar content of iron trichloride and ferric sulfate, the content 0.002～0.006g/ml of Sodium dodecylbenzene sulfonate in the aqueous solution;
(2) with presoma thermal treatment 0.5～3h under 250～400 ℃ of air atmospheres;
(3) then with the product that obtains at 300～450 ℃ of H
2Thermal treatment 1～3h under the atmosphere slowly cools to 150～250 ℃ at last, with atmosphere by H
2Change O into
2, thermal treatment 1～3h had both obtained final product.
2, method according to claim 1 is characterized in that, the crystalline phase of described product consists of γ-Fe
2O
3(JCPDS No.39-1346), pattern are nano-hollow sphere structured.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101552064B (en) * | 2008-12-16 | 2011-01-26 | 北京理工大学 | Method for preparing hollow magnetic ball |
| CN101704667B (en) * | 2009-11-13 | 2012-02-29 | 无锡泰达纺织科技有限公司 | Method for preparing magnetic ferrite hollow spheres used for removing microcystin |
| CN103011303A (en) * | 2013-01-07 | 2013-04-03 | 云南云天化股份有限公司 | Iron oxide particle and preparation method thereof as well as electrorheological fluid |
| CN103288139A (en) * | 2013-05-08 | 2013-09-11 | 北京工业大学 | Method for preparing alpha-Fe2O3 hollow structure and alpha-Fe2O3/K1.33Mn8O16 nanowire |
| CN103726090A (en) * | 2012-10-11 | 2014-04-16 | 中国科学院大连化学物理研究所 | Preparation method for alpha-Fe2O3 photoanode applied to photoelectrolysis |
| CN106366525A (en) * | 2016-11-03 | 2017-02-01 | 中国海洋大学 | Ultraviolet shielding composite membrane and preparation method thereof |
| CN107354480A (en) * | 2017-06-19 | 2017-11-17 | 汕头大学 | A kind of metal oxide/NiPi light anodes material and its preparation |
| WO2018187926A1 (en) * | 2017-04-11 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Method for preparing fe2o3 having hollow structure based on oil bath synthesis |
| CN109338466A (en) * | 2018-09-02 | 2019-02-15 | 景德镇陶瓷大学 | It is a kind of to prepare monocrystalline Fe2O3The method of nano-particles self assemble elliptical shape ball micro nano structure |
| CN114606527A (en) * | 2022-04-06 | 2022-06-10 | 齐鲁工业大学 | One-dimensional defective iron oxide nanorod visible light anode and preparation method and application thereof |
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2008
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101552064B (en) * | 2008-12-16 | 2011-01-26 | 北京理工大学 | Method for preparing hollow magnetic ball |
| CN101704667B (en) * | 2009-11-13 | 2012-02-29 | 无锡泰达纺织科技有限公司 | Method for preparing magnetic ferrite hollow spheres used for removing microcystin |
| CN103726090A (en) * | 2012-10-11 | 2014-04-16 | 中国科学院大连化学物理研究所 | Preparation method for alpha-Fe2O3 photoanode applied to photoelectrolysis |
| CN103011303B (en) * | 2013-01-07 | 2014-12-03 | 云南云天化股份有限公司 | Preparation method of iron oxide particle |
| CN103011303A (en) * | 2013-01-07 | 2013-04-03 | 云南云天化股份有限公司 | Iron oxide particle and preparation method thereof as well as electrorheological fluid |
| CN103288139A (en) * | 2013-05-08 | 2013-09-11 | 北京工业大学 | Method for preparing alpha-Fe2O3 hollow structure and alpha-Fe2O3/K1.33Mn8O16 nanowire |
| CN103288139B (en) * | 2013-05-08 | 2014-11-26 | 北京工业大学 | Method for preparing alpha-Fe2O3 hollow structure and alpha-Fe2O3/K1.33Mn8O16 nanowire |
| CN106366525A (en) * | 2016-11-03 | 2017-02-01 | 中国海洋大学 | Ultraviolet shielding composite membrane and preparation method thereof |
| WO2018187926A1 (en) * | 2017-04-11 | 2018-10-18 | 深圳市佩成科技有限责任公司 | Method for preparing fe2o3 having hollow structure based on oil bath synthesis |
| CN107354480A (en) * | 2017-06-19 | 2017-11-17 | 汕头大学 | A kind of metal oxide/NiPi light anodes material and its preparation |
| CN107354480B (en) * | 2017-06-19 | 2019-03-01 | 汕头大学 | A kind of metal oxide/NiPi optical anode material and its preparation |
| CN109338466A (en) * | 2018-09-02 | 2019-02-15 | 景德镇陶瓷大学 | It is a kind of to prepare monocrystalline Fe2O3The method of nano-particles self assemble elliptical shape ball micro nano structure |
| CN114606527A (en) * | 2022-04-06 | 2022-06-10 | 齐鲁工业大学 | One-dimensional defective iron oxide nanorod visible light anode and preparation method and application thereof |
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|---|---|
| CN101318709B (en) | 2011-04-06 |
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