CN103482708A - Method of preparing monodisperse iron oxide quasi-cubic mesoscopic crystal with adjustable grain size - Google Patents
Method of preparing monodisperse iron oxide quasi-cubic mesoscopic crystal with adjustable grain size Download PDFInfo
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Abstract
The invention discloses a method of preparing a monodisperse iron oxide quasi-cubic mesoscopic crystal with an adjustable grain size. The method comprises the following steps: firstly, dissolving iron trichloride in aqueous liquor of alcohol; and then, transferring the liquor into a solvothermal device for carrying out solvothermal reaction, and centrifuging and drying the obtained substance to obtain the iron oxide quasi-cubic mesoscopic crystal. The grain size of the iron oxide quasi-cubic mesoscopic crystal can be adjusted by changing the concentration of the aqueous liquor of the alcohol. The method disclosed by the invention is simple in process, short in reaction time, low in cost, simple in needed equipment and easy to synthesize on large scale; the prepared iron oxide quasi-cubic mesoscopic crystal has good crystallinity and is continuously adjustable in grain size within a range of 300 nm-2 mu m.
Description
Technical field
The present invention relates to a kind of method for preparing the accurate cube of sight crystal that is situated between of single dispersing iron oxide, especially prepare the method that accurate cube of Jie of the adjustable single dispersing iron oxide of particle diameter sees crystal.
Background technology
α-Fe
2o
3be a kind of cheap, corrosion-resistant, eco-friendly semi-conductor, be widely used in catalysis, gas sensing, the fields such as electrochemistry.Various ferric oxide nano structures are synthesized out.Wherein, it is especially noticeable that accurate cubic structure Jie of single dispersing iron oxide that the method for employing forced hydrolysis synthesizes sees crystal.The synthesis strategy of employing " from top to bottom ", accurate cube of sight crystal that is situated between of ferric oxide can be used as the initial feed that synthetic various different-shape ferric oxide Jie sees crystal.Therefore, the researchist needs to regulate the particle diameter of the accurate cube of sight crystal that is situated between of single dispersing iron oxide.
In monodisperse system, the particle diameter of particle is mainly to control by number of nuclei.In the past, the researchist adopts the concentration of controlling iron ion in solution, the pH in nucleation process, and temperature is controlled the particle diameter of the accurate cube of sight crystal that is situated between of ferric oxide.Yet Jie of preparation sees crystal at a lower temperature usually needs the ageing time of a couple of days; And under comparatively high temps, preparation Jie sight crystal required time is shorter, but particle size is too small.Therefore need to develop a kind of novel method, can either can in a big way, regulate and control to be situated between to see the size of crystal again by Reaction time shorten.
Summary of the invention
The purpose of this invention is to provide a kind of technique simple, the method for preparing the accurate cube of sight crystal that is situated between of the adjustable single dispersing iron oxide of particle diameter that the reaction times is short.
The method for preparing the accurate cube of sight crystal that is situated between of the adjustable single dispersing iron oxide of particle diameter of the present invention comprises the following steps:
1) iron trichloride is dissolved in the pure aqueous solution, the volumetric molar concentration of alcohol is 0.01 ~ 17 M, and the volumetric molar concentration of iron trichloride in solution is 0.01 ~ 1 M;
2) solution step 1) made is transferred in the solvent thermal device, carries out solvent thermal reaction 5 min～6 h under 100 ~ 240 ℃, centrifugal, drying.
Above-mentioned iron trichloride can be FERRIC CHLORIDE ANHYDROUS or Iron(III) chloride hexahydrate.Described alcohol can be one or more of methyl alcohol, ethanol, propyl alcohol, Virahol and butanols.
Accurate cube of ferric oxide prepared by the present invention is situated between the particle diameter of seeing crystal can be by changing pure volumetric molar concentration and the solvent thermal reaction condition is regulated.
Technique of the present invention is simple, and the reaction times is short, and cost is low, and required equipment is simple, easily extensive synthetic, and accurate cube of Jie of the ferric oxide made sees the good crystallinity of crystal, and particle diameter is adjustable continuously in 300 nm-2 μ m scope.
The accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the accurate cube of sight crystal that is situated between of the ferric oxide of embodiment 1.
Fig. 2 is the stereoscan photograph of the accurate cube of sight crystal that is situated between of embodiment 1 ferric oxide.
Fig. 3 is transmission electron microscope photo and the corresponding selected area electron diffraction style that accurate cube of embodiment 1 ferric oxide is situated between and sees crystal.
Fig. 4 is the stereoscan photograph of the accurate cube of sight crystal that is situated between of embodiment 2 ferric oxide.
Embodiment
Embodiment 1
1) 0.71 g FERRIC CHLORIDE ANHYDROUS is dissolved in the aqueous solution of 70 ml ethanol, the volumetric molar concentration of ethanol is 2.45 M.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 30 min under 200 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains accurate cube of ferric oxide and is situated between and sees crystal.
The X ray diffracting spectrum of the accurate cube of sight crystal that is situated between of the ferric oxide of preparation is as shown in Fig. 1, and its diffraction peak is consistent with the standard diagram of rhombohedral iron ore (hematite) ferric oxide, illustrates that products obtained therefrom is the rhombohedral iron ore ferric oxide.By the Scherrer formula, calculate, its crystal mean diameter is 40 nm.The stereoscan photograph of the accurate cube of sight crystal that is situated between of the ferric oxide that Fig. 2 is the preparation of this example, accurate cube of median size of seeing crystal that is situated between of ferric oxide is about 600 nm as we can see from the figure.Accurate cube of transmission electron microscope photo and corresponding selected area electron diffraction style that is situated between and sees crystal of the ferric oxide that Fig. 3 is the preparation of this example.As can be seen from the figure, accurate cube of sight crystal that is situated between of ferric oxide has the structure of single crystal-like, is situated between and sees crystalline structure.
Embodiment 2
1) 0.71 g FERRIC CHLORIDE ANHYDROUS is dissolved in the aqueous solution of 70 ml alcohol, the volumetric molar concentration of ethanol is 12.25 M.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 6 h under 150 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains accurate cube of ferric oxide and is situated between and sees crystal.
The stereoscan photograph of the accurate cube of sight crystal that is situated between of the ferric oxide of preparation is as shown in Fig. 4, and its median size is about 1.5 μ m as we can see from the figure.
Embodiment 3 ~ embodiment 8
Step is with embodiment 2, and difference is the volumetric molar concentration different (in Table 1) of ethanol, and from table 1, accurate cube of particle diameter of seeing crystal that is situated between of ferric oxide changes along with the variation of alcohol concn.
Table 1
Embodiment 9
1) 0.71 g FERRIC CHLORIDE ANHYDROUS is dissolved in the aqueous solution of 70 ml alcohol, the volumetric molar concentration of ethanol is 17 M.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 12 h under 150 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains accurate cube of ferric oxide and is situated between and sees crystal, and its median size is for being 1.8 μ m.
Embodiment 10
1) 0.71 g FERRIC CHLORIDE ANHYDROUS is dissolved in the aqueous solution of 70 ml alcohol, the volumetric molar concentration of ethanol is 12.25 M.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 6 h under 100 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains accurate cube of ferric oxide and is situated between and sees crystal, its median size 2 μ m.
Embodiment 11
1) 0.71 g FERRIC CHLORIDE ANHYDROUS is dissolved in the aqueous solution of 70 ml alcohol, the volumetric molar concentration of ethanol is 12.25 M.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 5 min under 240 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains accurate cube of ferric oxide and is situated between and sees crystal, its median size 300 nm.
Claims (3)
1. one kind prepares the method that accurate cube of Jie of the adjustable single dispersing iron oxide of particle diameter sees crystal, it is characterized in that comprising the following steps:
1) iron trichloride is dissolved in the pure aqueous solution, the volumetric molar concentration of alcohol is 0.01 ~ 17 M, and the volumetric molar concentration of iron trichloride in solution is 0.01 ~ 1 M;
2) solution step 1) made is transferred in the solvent thermal device, carries out solvent thermal reaction 5 min～6 h under 100 ~ 240 ℃, centrifugal, drying.
2. according to the described method for preparing the accurate cube of sight crystal that is situated between of the adjustable single dispersing iron oxide of particle diameter of claim 1, it is characterized in that described iron trichloride is FERRIC CHLORIDE ANHYDROUS or Iron(III) chloride hexahydrate.
3. according to the described method for preparing the accurate cube of sight crystal that is situated between of the adjustable single dispersing iron oxide of particle diameter of claim 1, it is characterized in that described alcohol is one or more of methyl alcohol, ethanol, propyl alcohol, Virahol and butanols.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104815658A (en) * | 2015-04-09 | 2015-08-05 | 太原理工大学 | Tetrahexahedron iron oxide nanocrystalline catalyst, preparation method and application thereof |
| CN105002552A (en) * | 2014-04-15 | 2015-10-28 | 昆明仁旺科技有限公司 | Iridium mesoscopic crystal synthesis method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60246225A (en) * | 1984-05-21 | 1985-12-05 | Hisanori Bando | Ferric oxide particle powder and its production |
| CN101293674A (en) * | 2008-06-12 | 2008-10-29 | 浙江大学 | Method for preparing spindle shaped alpha-Fe2O3 powder |
| CN102603012A (en) * | 2012-03-13 | 2012-07-25 | 中国科学院山西煤炭化学研究所 | Preparation method of nano iron oxide with good solvent dispersity |
-
2013
- 2013-09-06 CN CN201310402020.7A patent/CN103482708A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60246225A (en) * | 1984-05-21 | 1985-12-05 | Hisanori Bando | Ferric oxide particle powder and its production |
| CN101293674A (en) * | 2008-06-12 | 2008-10-29 | 浙江大学 | Method for preparing spindle shaped alpha-Fe2O3 powder |
| CN102603012A (en) * | 2012-03-13 | 2012-07-25 | 中国科学院山西煤炭化学研究所 | Preparation method of nano iron oxide with good solvent dispersity |
Non-Patent Citations (2)
| Title |
|---|
| SHUAI HE ET AL.: "Facile Size-Controllable Synthesis of Colorful Quasi-Cubic -Fe2O3 Materials from Nanoscale to Microscale and Their Properties Related to the Size Effect", 《CHEMPLUSCHEM》, vol. 78, 28 June 2013 (2013-06-28), pages 875 - 883 * |
| 许慧丽等: "不同形貌的α-Fe2O3的水热控制合成", 《浙江大学学报》, vol. 35, no. 5, 30 September 2008 (2008-09-30), pages 546 - 549 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105002552A (en) * | 2014-04-15 | 2015-10-28 | 昆明仁旺科技有限公司 | Iridium mesoscopic crystal synthesis method |
| CN104815658A (en) * | 2015-04-09 | 2015-08-05 | 太原理工大学 | Tetrahexahedron iron oxide nanocrystalline catalyst, preparation method and application thereof |
| CN104815658B (en) * | 2015-04-09 | 2017-04-12 | 太原理工大学 | Tetrahexahedron iron oxide nanocrystalline catalyst, preparation method and application thereof |
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