CN101318709B - 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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- CN101318709B CN101318709B CN2008100394915A CN200810039491A CN101318709B CN 101318709 B CN101318709 B CN 101318709B CN 2008100394915 A CN2008100394915 A CN 2008100394915A CN 200810039491 A CN200810039491 A CN 200810039491A CN 101318709 B CN101318709 B CN 101318709B
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000004005 microsphere Substances 0.000 title claims abstract description 6
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 title abstract 2
- 239000000047 product Substances 0.000 claims abstract description 16
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012467 final product Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- 238000007669 thermal treatment Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 14
- 229910001566 austenite Inorganic materials 0.000 claims description 12
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 10
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 abstract description 6
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 3
- 239000002243 precursor Substances 0.000 abstract 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 229910006540 α-FeOOH Inorganic materials 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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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 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 washing to produce an alpha-FeOOH precursor. The precursor is subject to a heat treatment for 0.5 to 3 hours under an air atmosphere between 250 and 400 DEG C, then the obtained product is subject to the heat treatment for 1 to 3 hours under an H2 atmosphere 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 obtained 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 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 promptly obtains final product.
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 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 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.
Embodiment 2
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,, put 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. one kind prepares 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 promptly obtains final product.
2. method according to claim 1 is characterized in that the crystalline phase of described product consists of γ-Fe
2O
3, pattern is nano-hollow sphere structured.
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|---|---|---|---|
| CN2008100394915A CN101318709B (en) | 2008-06-25 | 2008-06-25 | Method for preparing nano-gamma-Fe2O3 hollow magnetic microsphere |
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|---|---|---|---|
| CN2008100394915A CN101318709B (en) | 2008-06-25 | 2008-06-25 | Method for preparing nano-gamma-Fe2O3 hollow magnetic microsphere |
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| CN101318709A CN101318709A (en) | 2008-12-10 |
| CN101318709B true CN101318709B (en) | 2011-04-06 |
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Families Citing this family (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 |
| 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 |
| 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 |
| CN107354480B (en) * | 2017-06-19 | 2019-03-01 | 汕头大学 | A kind of metal oxide/NiPi optical anode material and its preparation |
| CN109338466B (en) * | 2018-09-02 | 2020-05-05 | 景德镇陶瓷大学 | Preparation of single crystal Fe2O3Method for self-assembling nano-particle into elliptical micro-nano structure |
| CN114606527B (en) * | 2022-04-06 | 2023-05-12 | 齐鲁工业大学 | One-dimensional defective ferric oxide nano rod visible light anode and preparation method and application thereof |
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