CN103172124B - Method for preparing ferric oxide three-dimensional nanostructure through solid-state chemical reaction - Google Patents
Method for preparing ferric oxide three-dimensional nanostructure through solid-state chemical reaction Download PDFInfo
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- CN103172124B CN103172124B CN201310132409.4A CN201310132409A CN103172124B CN 103172124 B CN103172124 B CN 103172124B CN 201310132409 A CN201310132409 A CN 201310132409A CN 103172124 B CN103172124 B CN 103172124B
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- ferric oxide
- dimensional nanostructure
- sodium
- solid state
- state reaction
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Abstract
The invention provides a method for preparing a ferric oxide three-dimensional nanostructure through solid-state chemical reaction. The ferric oxide three-dimensional nanostructure is prepared from ferric salt or ferrous salt and a reducing agent, which are subjected to solid-state chemical reaction through by grinding or ball-milling, and then are subjected to aftertreatment. In the reaction process, a surfactant can be added to promote formation of the three-dimensional nanostructure product. The method has the advantages that the raw materials are cheap and easily available; the reaction operation is simple, little time is cost, and the volume production of nanostructures is easy; and the ferric oxide three-dimensional nanostructure prepared by the method has big specific surface area, can be applied to excellent gas sensitive, adsorbing, catalytic, electrode and carrier materials and has extensive application prospect.
Description
Technical field
The present invention relates to a kind of method of preparing ferric oxide three-dimensional nanostructure by solid state reaction, belong to nano material synthesis technical field.
Background technology
Nano-sized iron oxide (the Fe of different crystalline phases
3o
4, γ-Fe
2o
3, α-Fe
2o
3) be widely used in multiple fields owing to thering is different characteristics.Nanometer Fe
3o
4and γ-Fe
2o
3there is magnetic and good biocompatibility, can be widely used in the fields such as target drug-carrying, medical imaging, magnetic storage and catalysis; Nanometer α-Fe
2o
3have n-N-type semiconductorN characteristic and high stability, it has important application in fields such as sensor, lithium ion battery, catalysis.As everyone knows, the pattern of nano material has material impact to its character, and the three-dimensional hierarchical structure nano-sized iron oxide being made up of the structure primitive (as nanoparticle, nanometer rod, nanotube, nano wire, nanometer sheet etc.) of low-dimensional nano structure causes investigator's extensive concern owing to having the specific surface area of superelevation with the special performance relevant to its pattern.
At present, reported the preparation of several different methods for ferric oxide three-dimensional nanostructure.As first the people such as L. Wan make the precursor of iron content in the ethylene glycol refluxing, afterwards this precursor is heat-treated at different atmosphere and temperature, obtain respectively having the nanometer Fe of three-dimensional flower-shaped structure
3o
4, nanometer γ-Fe
2o
3with nanometer α-Fe
2o
3(Advanced Materials, 18 volumes, 2426-2431 page, 2006).L. the people such as Zhang, by the booster action of microwave irradiation, adds block polymer in ethylene glycol, has synthesized rose-shaped nanometer Fe by iron(ic) chloride and sodium-acetate
3o
4(The Journal of Physical Chemistry C, 114 volumes, 6237-6242 page, 2010).T. first the people such as Fei has synthesized FeOOH precursor by solvent-thermal method, afterwards it is calcined, and has made flower-shaped α-Fe
2o
3hierarchy (ACS Applied Materials & Interfaces, 3 volumes, 4689-4694 page, 2011).Can find out, although these ferric oxide three-dimensional nanostructures have the excellent performance such as air-sensitive and absorption, but for the preparation of the synthetic method more complicated of these hierarchies, react higher to equipment requirements, be unfavorable for industry's enlarging production, this has limited the widespread use in practice of ferric oxide classification nanostructure.
Given this, in order to realize the more simply preparation to ferric oxide three-dimensional nanostructure, thereby be effectively applied in every field, be necessary to develop the preparation method that a kind of technique is simple, easy to operate, be easy to realize amplification production.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing ferric oxide three-dimensional nanostructure.The method, by using cheap raw material, adopts simple operation method, can synthesize the different sorts ferric oxide with three-dimensional classification nanostructure through solid state reaction.
Technical scheme of the present invention is as follows:
Solid state reaction is prepared a method for ferric oxide three-dimensional nanostructure, and it comprises the following steps: the ratio that is 0.1 ~ 10:1 with reductive agent according to mol ratio by molysite or ferrous salt is mixed; Can add tensio-active agent, the mass ratio of molysite or ferrous salt and tensio-active agent is 0.1 ~ 10:1; Grind or ball-milling reaction 20 ~ 60 minutes; Product is water, washing with alcohol respectively, 20 ~ 120
oc air drying 0.5 ~ 24 hour; Dried sample is in air atmosphere 200 ~ 600
oc heat-treats 1 ~ 5 hour, finally obtains ferric oxide three-dimensional nanostructure.
Molysite of the present invention or ferrous salt are one or more in ferric iron or ferrous acetate, nitrate, vitriol or muriate.Described reductive agent is the reductive agent of solid form, comprises one or more in sodium borohydride, POTASSIUM BOROHYDRIDE, azanol, oxammonium hydrochloride, sodium hypophosphite, Trisodium Citrate, sodium oxalate, hydrazonium sulfate, glucose, xitix, citric acid, oxalic acid, amino acid etc.Described tensio-active agent agent is one or more in polyoxyethylene glycol, polyvinylpyrrolidone, sodium polystyrene sulfonate, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, sodium cetanesulfonate, cetyl trimethylammonium bromide, ethylenediamine tetraacetic acid (EDTA) etc.The hierarchy of prepared ferric oxide three-dimensional nanostructure for being made up of ultrathin nanometer sheet, comprises Fe
3o
43-D nano, structure, γ-Fe
2o
33-D nano, structure, α-Fe
2o
33-D nano, structure.
Compared with prior art, the present invention has the following advantages: taking solid state reaction as basis, adopt raw material cheap and easy to get, by simple grinding or ball milling operation, then pass through suitable thermal treatment, can make and comprise Fe
3o
4, γ-Fe
2o
3and α-Fe
2o
3in interior ferric oxide three-dimensional nanostructure.Preparation method is simple, and product yield is high, is easy to realize the features such as production in enormous quantities and all makes the present invention have very wide application prospect.
Brief description of the drawings
Fig. 1 is Fe prepared by first embodiment of the invention
3o
4the transmission electron microscope photo of 3-D nano, structure.
Fig. 2 is α-Fe prepared by second embodiment of the invention
2o
3the transmission electron microscope photo of 3-D nano, structure.
Fig. 3 is Fe prepared by third embodiment of the invention
3o
4the transmission electron microscope photo of 3-D nano, structure.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.These embodiment are interpreted as being only not used in and limiting the scope of the invention for the present invention is described.After having read the content of the present invention's record, the various changes of the present invention being made based on principle of the present invention or amendment fall into the claims in the present invention book limited range equally.
Embodiment mono-:
Get the FeCl of 3 mmol
24H
2o(0.60 g) with the NaBH of 6 mmol
4(0.23 g), at room temperature carries out griding reaction 40 minutes, and product water, washing with alcohol, 60
oc air drying 5 hours, obtains Fe as shown in Figure 1
3o
43-D nano, structure.
Embodiment bis-:
Get the FeCl of 3 mmol
24H
2o(0.60 g) with the NaBH of 6 mmol
4(0.23 g), then adds 0.87 g sodium lauryl sulphate, at room temperature carries out griding reaction 40 minutes, and product water, washing with alcohol, 20
oc air drying 24 hours, dried sample is in air atmosphere 600
oc thermal treatment 1 hour, obtains α-Fe as shown in Figure 2
2o
33-D nano, structure.
Embodiment tri-:
Get the FeCl of 3 mmol
36H
2o(0.81 g) with the NaBH of 9 mmol
4(0.34 g), at room temperature carries out griding reaction 40 minutes, and product water, washing with alcohol, 30
oc air drying 10 hours, obtains Fe as shown in Figure 3
3o
43-D nano, structure.
Claims (6)
1. a solid state reaction is prepared the method for ferric oxide three-dimensional nanostructure, it comprises the following steps: molysite or ferrous salt are mixed with reductive agent, can add tensio-active agent, grind or ball-milling reaction, product obtains final ferric oxide three-dimensional nanostructure after washing, dry and thermal treatment.
2. the method for preparing ferric oxide three-dimensional nanostructure according to a kind of solid state reaction claimed in claim 1, is characterized in that: the mol ratio of molysite or ferrous salt and reductive agent is 0.1 ~ 10:1; The mass ratio of molysite or ferrous salt and tensio-active agent is 0.1 ~ 10:1; The time of grinding or ball-milling reaction is 20 ~ 60 minutes; Product is water, washing with alcohol respectively, 20 ~ 120
oc air drying 0.5 ~ 24 hour; Dried sample is in air atmosphere 200 ~ 600
oc heat-treats 1 ~ 5 hour.
3. the method for preparing ferric oxide three-dimensional nanostructure according to a kind of solid state reaction claimed in claim 1, is characterized in that: the molysite using or ferrous salt are one or more in ferric iron or ferrous acetate, nitrate, vitriol or muriate.
4. prepare the method for ferric oxide three-dimensional nanostructure according to a kind of solid state reaction claimed in claim 1, it is characterized in that: the reductive agent that the reductive agent using is solid form, comprises one or more in sodium borohydride, POTASSIUM BOROHYDRIDE, azanol, oxammonium hydrochloride, sodium hypophosphite, Trisodium Citrate, sodium oxalate, hydrazonium sulfate, glucose, xitix, citric acid, oxalic acid, amino acid etc.
5. the method for preparing ferric oxide three-dimensional nanostructure according to a kind of solid state reaction claimed in claim 1, is characterized in that: the tensio-active agent using is one or more in polyoxyethylene glycol, polyvinylpyrrolidone, sodium polystyrene sulfonate, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, sodium cetanesulfonate, cetyl trimethylammonium bromide, ethylenediamine tetraacetic acid (EDTA) etc.
6. the method for preparing ferric oxide three-dimensional nanostructure according to a kind of solid state reaction claimed in claim 1, is characterized in that: the hierarchy of prepared ferric oxide three-dimensional nanostructure for being made up of ultrathin nanometer sheet, comprises Fe
3o
43-D nano, structure, γ-Fe
2o
33-D nano, structure, α-Fe
2o
33-D nano, structure.
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| CN103172124B true CN103172124B (en) | 2014-08-06 |
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| CN104402067B (en) * | 2014-12-05 | 2016-09-28 | 渤海大学 | A kind of method that directly high specific surface area and mesoporous metal-oxide is prepared in thermal decomposition |
| CN105798323B (en) * | 2016-03-18 | 2018-04-06 | 西北师范大学 | The method that ball milling assistant interface prepares bigger serface transition metal boron alloy material |
| CN105762354B (en) * | 2016-05-17 | 2018-04-13 | 安徽师范大学 | A kind of flower-shaped ferric oxide nano-material and preparation method thereof, negative electrode of lithium ion battery and lithium ion battery |
| CN106799232B (en) * | 2016-12-15 | 2019-08-06 | 浙江工业大学 | A kind of iron based ammonia synthesis catalyst and its preparation method and application of the Nanoscale Iron modification of solid state chemical reaction preparation |
| CN106927511B (en) * | 2017-04-17 | 2018-12-07 | 吉林大学 | A kind of high-energy ball milling preparation method of magnetic ferroferric oxide nanometer powder |
| CN107311238A (en) * | 2017-08-02 | 2017-11-03 | 浙江理工大学 | A kind of preparation method of the hollow ferroso-ferric oxide microballoon of superparamagnetic |
| CN107720808A (en) * | 2017-09-29 | 2018-02-23 | 张家港江苏科技大学产业技术研究院 | A kind of method of low temperature preparation high-purity Nano-class Asia titanium oxide |
| CN110038572A (en) * | 2019-04-30 | 2019-07-23 | 南开大学 | A kind of α-Fe for degradable organic pollutant2O3/ Fe photochemical catalyst and preparation method thereof |
| CN111235625B (en) * | 2020-01-21 | 2022-01-25 | 江苏理工学院 | Iron oxide single crystal nano spherical particle and molten salt method synthesis method thereof |
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