CN101913658A - Alpha type ferric oxide and preparation method thereof - Google Patents
Alpha type ferric oxide and preparation method thereof Download PDFInfo
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- CN101913658A CN101913658A CN 201010283476 CN201010283476A CN101913658A CN 101913658 A CN101913658 A CN 101913658A CN 201010283476 CN201010283476 CN 201010283476 CN 201010283476 A CN201010283476 A CN 201010283476A CN 101913658 A CN101913658 A CN 101913658A
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Abstract
The invention discloses an alpha type ferric oxide and a preparation method thereof, and relates to a metallic oxide. A method for preparing the alpha type ferric oxide which has uniform particle distribution and a columnar or flower-like structure with excellent magnetic property is provided. The method comprises the following steps of: preparing water-soluble potassium ferricyanide solution and sodium hydroxide solution respectively, and mixing the water-soluble potassium ferricyanide solution and the sodium hydroxide solution to obtain mixed liquid; adding a surfactant into the mixed liquid, and fully dissolving the surfactant after ultraphonic treatment to obtain light yellow settled solution; transferring the light yellow settled solution into a stainless steel reaction kettle, and heating for reaction; and after products generated from the heating for reaction are cooled to room temperature, performing centrifugal separation on precipitates at the bottom of the kettle, then cleaning the precipitates, and drying the obtained products so as to obtain the alpha type ferric oxide. When trisodium citrate is taken as the surfactant, alpha type ferric oxide particles with columnar structures can be prepared; and when urea is taken as the surfactant, the alpha type ferric oxide particles with flower-like structures can be prepared.
Description
Technical field
The present invention relates to a kind of metal oxide, especially relate to the alpha-type ferric oxide (α-Fe of a kind of column or flower-like structure
2O
3) and preparation method thereof.
Background technology
Alpha-type ferric oxide is a kind of important metal oxide, characteristic with n N-type semiconductorN, its band gap width is 2.2eV, has very strong absorption at visible region, with low cost in addition, it is widely used at aspects such as luster coating, plastics, electronics, magnetic recording material, catalyzer and biomedical engineerings.In addition, because it has higher gas sensing property, ferric oxide also can be used for detecting airborne inflammable gas and toxic gas.
The size of material, pattern, structure have bigger influence to its relevant performance.Pertinent literature (1, T.S.Zhang, P.Hing, R.F.Zhang.J.Mater.Sci, 2000,35,1419; 2, Sun Yuhan, Lv Baoliang, Wu Dong, Xu Yao. the non-template legal system is equipped with the method [P] of alpha-ferric oxide nano-rings. publication number: CN101264937A; 3, Sun Yuhan, Lv Baoliang, Wu Dong, Xu Yao. the non-template legal system is equipped with the method [P] of alpha-ferric oxide nanotube. publication number: CN101264936A) reported the ferric oxide of different dimensions, pattern and structure, as nanometer rod, nanotube, nano-rings, tiny balloon etc.Prepare the ferric oxide of tool ad hoc structure and study its correlated performance and use and become at present comparatively active research field.
Summary of the invention
Purpose of the present invention aims to provide a kind of even particle distribution, and has the column of superior magnetic property or the alpha-type ferric oxide (α-Fe of flower-like structure
2O
3) the preparation method.
The present invention includes following steps:
1) prepares water-soluble iron potassium cyanide solution and sodium hydroxide solution respectively, water-soluble iron potassium cyanide solution and sodium hydroxide solution are mixed, get mixed solution;
2) in mixed solution, add tensio-active agent, it fully dissolved after ultrasonic, faint yellow settled solution;
3) with step 2) the faint yellow settled solution of gained is transferred in the stainless steel cauldron temperature reaction;
4) treat that the product after the step 3) temperature reaction is cooled to room temperature,,, promptly get alpha-type ferric oxide the products therefrom drying with throw out centrifugation after scouring at the bottom of the still.
In step 1), described water-soluble iron potassium cyanide solution and sodium hydroxide solution mix, and can be that water-soluble iron potassium cyanide solution and sodium hydroxide solution equal-volume mix; The volumetric molar concentration of the Tripotassium iron hexacyanide of described mixed solution can be 0.05～0.10M, and the volumetric molar concentration of sodium hydroxide can be 0.10～0.15M.
In step 2) in, described tensio-active agent can adopt trisodium citrate or urea etc., and the volumetric molar concentration of described trisodium citrate can be 0.125～0.25M; The volumetric molar concentration of described urea can be 0.16～0.32M; The described ultransonic time can be 3～5min.
In step 3), described temperature reaction can be warming up to 180 ℃ of reactions under air-proof condition, and the time of reaction can be 12～24h.
In step 4), described washing can be adopted dehydrated alcohol and deionized water wash; Described exsiccant temperature can be 60～80 ℃, and the exsiccant time can be 8～12h.
When tensio-active agent adopts trisodium citrate, can make columnar structure alpha-type ferric oxide particle, when tensio-active agent adopts urea, can make flower-like structure alpha-type ferric oxide particle.
It is starting raw material that the present invention adopts the Tripotassium iron hexacyanide, pass through hydro-thermal reaction, under certain temperature and time, prepare column or flower-like structure alpha-type ferric oxide particle, prepared column of the present invention or flower-like structure alpha-type ferric oxide particle have output big, be evenly distributed, characteristics such as magnetic property is superior, and this method mild condition, technology is simple.
Description of drawings
Fig. 1 is the X-ray diffraction spectrogram of the columnar structure alpha-type ferric oxide of embodiment 1 preparation.In Fig. 1, X-coordinate is diffraction angle 2 θ (deg.), and ordinate zou is diffracted intensity Intensity (a.u.); From left to right, diffraction peak is followed successively by 012,104,110,113,024,116,122,214,300,1010 crystal faces.
Fig. 2 is the scanning electron microscope picture of the columnar structure alpha-type ferric oxide of embodiment 1 preparation.In Fig. 2, (a) be low range, scale is 10 μ m; (b) be high magnification, scale is 1 μ m.
Fig. 3 is the transmission electron microscope picture of the columnar structure alpha-type ferric oxide of embodiment 1 preparation.In Fig. 3, (a) scale is 1 μ m; (b) scale is 50nm; (c) scale is 5nm, and spacing of lattice d is 0.36nm.
Fig. 4 is the magnetic hysteresis loop figure of the columnar structure alpha-type ferric oxide of embodiment 1 preparation.In Fig. 4, X-coordinate is coercive force H (Oe), and ordinate zou is remanent magnetism M (emu/g).
Fig. 5 is the X-ray diffraction spectrogram of the flower-like structure alpha-type ferric oxide of embodiment 5 preparations.In Fig. 5, X-coordinate is diffraction angle 2 θ (deg.), and ordinate zou is diffracted intensity Intensity (a.u.); From left to right, diffraction peak is followed successively by 012,104,110,202,024,116,122,214,300,1010 crystal faces.
Fig. 6 is the scanning electron microscope picture of the flower-like structure alpha-type ferric oxide of embodiment 5 preparations.In Fig. 6, (a) be low range, scale is 3 μ m; (b) be high magnification, scale is 1 μ m.
Fig. 7 is the transmission electron microscope picture of the flower-like structure alpha-type ferric oxide of embodiment 5 preparations.In Fig. 7, (a) scale is 1 μ m; (b) scale is 20nm; (c) scale is 10nm, and spacing of lattice d is 0.27nm.
Fig. 8 is the magnetic hysteresis loop figure of the flower-like structure alpha-type ferric oxide of embodiment 5 preparations.In Fig. 8, X-coordinate is coercive force H (Oe), and ordinate zou is remanent magnetism M (emu/g).
Embodiment
Embodiment 1
(1) takes by weighing the Tripotassium iron hexacyanide of 0.33g (1mmol), it is dissolved in the deionized water of 10mL, stir it is fully dissolved; Take by weighing 0.12g (3mmol) sodium hydroxide, it is dissolved in the deionized water of 10mL, stir it is fully dissolved, then with itself and potassium ferricyanide solution mixing.The concentration of the Tripotassium iron hexacyanide is 0.05M in the mixed solution, and concentration sodium hydroxide is 0.15M.
(2) add the trisodium citrate of 1.035g (about 4mmol) in the mixed solution, behind the ultrasonic 5min it fully dissolved, faint yellow settled solution, the concentration of trisodium citrate is 0.20M in the mixed solution.
(3) in the teflon-lined stainless steel cauldron that is 50mL with the above-mentioned yellow settled solution capacity of being transferred to, seal and be warming up to 180 ℃ of insulation 12h.
(4) question response naturally cools to room temperature after fully, with throw out centrifugation at the bottom of the still, and with dehydrated alcohol and deionized water wash 2～3 times, products therefrom is placed 60 ℃ of dry 12h, promptly gets columnar structure alpha-type ferric oxide particle.
Fig. 1 is the X-ray diffraction spectrogram of the product for preparing under embodiment 1 condition.With the pairing spacing of main diffraction peak in the spectrogram and diffraction peak relative intensity and 89-0598 number comparison one by one of PDF card, can determine that this product is purified α-Fe
2O
3Rhombohedral iron ore.
Fig. 2 is the scanning electron microscope shape appearance figure of the product for preparing under embodiment 1 condition.Zhi Bei α-Fe as seen from the figure
2O
3Particle is columnar structure, and is staggered, and favorable dispersity, long axis direction are about 1～5 μ m, and short-axis direction is about 0.5～3 μ m.
Fig. 3 is the transmission electron microscope shape appearance figure of the product for preparing under embodiment 1 condition.Zhi Bei columnar structure α-Fe as seen from the figure
2O
3The particle long axis direction is about 3.3 μ m, and short-axis direction is about 1.8 μ m.The observed spacing of lattice of high resolution picture is 0.36nm, corresponding to α-Fe
2O
3Particulate (012) crystal face.
Fig. 4 is the magnetic hysteresis loop figure of the product for preparing under embodiment 1 condition.Zhi Bei α-Fe as seen from the figure
2O
3Particulate remanent magnetism and coercive force are respectively 0.0529emu/g and 1951.36Oe.
Embodiment 2
(1) take by weighing 0.33g (1mmol) Tripotassium iron hexacyanide, it is dissolved in the deionized water of 10mL, stirring is fully dissolved it; Take by weighing 0.08g (2mmol) sodium hydroxide, it is dissolved in the deionized water of 10mL, stir it is fully dissolved, then with itself and potassium ferricyanide solution mixing.The concentration of the Tripotassium iron hexacyanide is 0.05M in the mixed solution, and concentration sodium hydroxide is 0.10M.
(2) add the trisodium citrate of 0.776g (3mmol) in the mixed solution, behind the ultrasonic 5min it fully dissolved, faint yellow settled solution, the concentration of trisodium citrate is 0.15M in the mixed solution.
(3) in the teflon-lined stainless steel cauldron that is 50mL with the above-mentioned yellow settled solution capacity of being transferred to, seal and be warming up to 180 ℃ of insulation 16h.
(4) with embodiment 1.
Embodiment 3
(1) with embodiment 1.
(2) add the trisodium citrate of 1.294g (5mmol) in the mixed solution, behind the ultrasonic 5min it fully dissolved, faint yellow settled solution, the concentration of trisodium citrate is 0.25M in the mixed solution.
(3) in the teflon-lined stainless steel cauldron that is 50mL with the above-mentioned yellow settled solution capacity of being transferred to, seal and be warming up to 180 ℃ of insulation 16h.
(4) with embodiment 1.
Embodiment 4
(1) take by weighing 0.66g (2mmol) Tripotassium iron hexacyanide, it is dissolved in the deionized water of 10mL, stirring is fully dissolved it; Take by weighing 0.08g (2mmol) sodium hydroxide, it is dissolved in the deionized water of 10mL, stir it is fully dissolved, then with itself and potassium ferricyanide solution mixing.The concentration of the Tripotassium iron hexacyanide is 0.10M in the mixed solution, and concentration sodium hydroxide is 0.10M.
(2) add the trisodium citrate of 0.647g (2.5mmol) in the mixed solution, behind the ultrasonic 3min it fully dissolved, faint yellow settled solution, the concentration of trisodium citrate is 0.125M in the mixed solution.
(3) with embodiment 1.
(4) question response naturally cools to room temperature after fully, with throw out centrifugation at the bottom of the still, and with dehydrated alcohol and deionized water wash 2～3 times, products therefrom is placed 60 ℃ of dry 12h.
(1) takes by weighing the Tripotassium iron hexacyanide of 0.33g (1mmol), it is dissolved in the deionized water of 10mL, stir it is fully dissolved; Take by weighing 0.12g (3mmol) sodium hydroxide, it is dissolved in the deionized water of 10mL, stir it is fully dissolved, then with itself and potassium ferricyanide solution mixing.The concentration of the Tripotassium iron hexacyanide is 0.05M in the mixed solution, and concentration sodium hydroxide is 0.15M.
(2) add the urea of 0.384g (6.4mmol) in the mixed solution, behind the ultrasonic 5min it fully dissolved, faint yellow settled solution, the concentration of urea is 0.32M in the mixed solution.
(3) in the teflon-lined stainless steel cauldron that is 50mL with the above-mentioned yellow settled solution capacity of being transferred to, seal and be warming up to 180 ℃ of insulation 12h.
(4) question response naturally cools to room temperature after fully, with throw out centrifugation at the bottom of the still, and with dehydrated alcohol and deionized water wash 2～3 times, products therefrom is placed 60 ℃ of dry 12h, promptly gets the alpha-type ferric oxide that size is about the flower-like structure of 5 μ m.
Fig. 5 is the X-ray diffraction spectrogram of the product for preparing under embodiment 5 conditions.With the pairing spacing of main diffraction peak in the spectrogram and diffraction peak relative intensity and 24-0072 number comparison one by one of PDF card, can determine that this product is purified α-Fe
2O
3Rhombohedral iron ore.
Fig. 6 is the scanning electron microscope shape appearance figure of the product for preparing under embodiment 5 conditions.Zhi Bei α-Fe as seen from the figure
2O
3Particles dispersed is good, and size is about 4～6 μ m.The flower-like structure of the visible gained of sem photograph under the high magnification is that the platy structure by many similar petals assembles, and the microplate size is about 2 μ m, and thickness is about 300nm.
Fig. 7 is the transmission electron microscope shape appearance figure of the product for preparing under embodiment 5 conditions.α-the Fe of Zhi Bei single flower-like structure as seen from the figure
2O
3Granular size is about 5 μ m.The observed spacing of lattice of high resolution picture is 0.27nm, corresponding to α-Fe
2O
3Particulate (104) crystal face.
Fig. 8 is the magnetic hysteresis loop figure of the product for preparing under embodiment 5 conditions.Zhi Bei α-Fe as seen from the figure
2O
3Particulate remanent magnetism and coercive force are respectively 0.047emu/g and 1415.36Oe.
Embodiment 6
(1) takes by weighing the Tripotassium iron hexacyanide of 0.33g (1mmol), it is dissolved in the deionized water of 10mL, stir it is fully dissolved; Take by weighing 0.08g (2mmol) sodium hydroxide, it is dissolved in the deionized water of 10mL, stir it is fully dissolved, then with itself and potassium ferricyanide solution mixing.The concentration of the Tripotassium iron hexacyanide is 0.05M in the mixed solution, and concentration sodium hydroxide is 0.10M.
(2) with embodiment 5.
(3) in the teflon-lined stainless steel cauldron that the above-mentioned yellow settled solution capacity of being transferred to is 50mL, seal and be warming up to 180 ℃ of insulation 16h.
(4) with embodiment 5.
Embodiment 7
(1) take by weighing 0.66g (2mmol) Tripotassium iron hexacyanide, it is dissolved in the deionized water of 10mL, stirring is fully dissolved it; Take by weighing 0.08g (2mmol) sodium hydroxide, it is dissolved in the deionized water of 10mL, stir it is fully dissolved, then with itself and potassium ferricyanide solution mixing.The concentration of the Tripotassium iron hexacyanide is 0.10M in the mixed solution, and concentration sodium hydroxide is 0.10M.
(2) add the urea of 0.192g (about 3.2mmol) in the mixed solution, behind the ultrasonic 5min it fully dissolved, faint yellow settled solution, the concentration of urea is 0.16M in the mixed solution.
(3) in the teflon-lined stainless steel cauldron that is 50mL with the above-mentioned yellow settled solution capacity of being transferred to, seal and be warming up to 180 ℃ of insulation 16h.
(4) with embodiment 5.
Embodiment 8
(1) with embodiment 5.
(2) add the urea of 0.288g (4.8mmol) in the mixed solution, behind the ultrasonic 5min it fully dissolved, faint yellow settled solution, the concentration of urea is 0.24M in the mixed solution.
(3) with embodiment 5.
(4) question response naturally cools to room temperature after fully, with throw out centrifugation at the bottom of the still, and with dehydrated alcohol and deionized water wash 2～3 times, products therefrom is placed 60 ℃ of dry 10h.
Claims (9)
1. the preparation method of an alpha-type ferric oxide is characterized in that may further comprise the steps:
1) prepares water-soluble iron potassium cyanide solution and sodium hydroxide solution respectively, water-soluble iron potassium cyanide solution and sodium hydroxide solution are mixed, get mixed solution;
2) in mixed solution, add tensio-active agent, it fully dissolved after ultrasonic, faint yellow settled solution;
3) with step 2) the faint yellow settled solution of gained is transferred in the stainless steel cauldron temperature reaction;
4) treat that the product after the step 3) temperature reaction is cooled to room temperature,,, promptly get alpha-type ferric oxide the products therefrom drying with throw out centrifugation after scouring at the bottom of the still.
2. the preparation method of a kind of alpha-type ferric oxide as claimed in claim 1 is characterized in that in step 1), and described water-soluble iron potassium cyanide solution and sodium hydroxide solution mix, and is that water-soluble iron potassium cyanide solution and sodium hydroxide solution equal-volume mix.
3. the preparation method of a kind of alpha-type ferric oxide as claimed in claim 1 is characterized in that in step 1), and the volumetric molar concentration of the Tripotassium iron hexacyanide of described mixed solution is 0.05～0.10M, and the volumetric molar concentration of sodium hydroxide is 0.10～0.15M.
4. the preparation method of a kind of alpha-type ferric oxide as claimed in claim 1 is characterized in that in step 2) in, described tensio-active agent is trisodium citrate or urea.
5. the preparation method of a kind of alpha-type ferric oxide as claimed in claim 4, the volumetric molar concentration that it is characterized in that described trisodium citrate is 0.125～0.25M; The volumetric molar concentration of described urea is 0.16～0.32M.
6. the preparation method of a kind of alpha-type ferric oxide as claimed in claim 1 is characterized in that in step 2) in, the described ultransonic time is 3～5min.
7. the preparation method of a kind of alpha-type ferric oxide as claimed in claim 1 is characterized in that in step 3), and described temperature reaction is under air-proof condition, is warming up to 180 ℃ of reactions, and the time of reaction is 12～24h.
8. the preparation method of a kind of alpha-type ferric oxide as claimed in claim 1 is characterized in that in step 4), and described washing is to adopt dehydrated alcohol and deionized water wash.
9. the preparation method of a kind of alpha-type ferric oxide as claimed in claim 1 is characterized in that in step 4), and described exsiccant temperature is 60～80 ℃, and the exsiccant time is 8～12h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352134A (en) * | 2011-08-23 | 2012-02-15 | 华南理工大学 | Method for preparing nanometer ferric oxide water-soluble powder |
| CN102674471A (en) * | 2012-04-16 | 2012-09-19 | 北京航空航天大学 | Preparation method of flower-like mesoporous ferric oxide nano-material |
| CN102826612A (en) * | 2012-09-24 | 2012-12-19 | 厦门大学 | Preparation method of three-dimensional flower-shaped structure alpha-type ferric oxide |
| CN103204550A (en) * | 2013-04-12 | 2013-07-17 | 陕西科技大学 | Controllable preparation method of micron-order Fe2O3 |
| CN103464740A (en) * | 2013-08-16 | 2013-12-25 | 安徽师范大学 | Micro and nano alpha-Fe2O3 material and preparation method thereof |
| CN103771533A (en) * | 2014-01-24 | 2014-05-07 | 天津理工大学 | Preparation method of alpha-Fe2O3 microsphere with flower-like hierarchical structure |
| CN104773743A (en) * | 2015-04-10 | 2015-07-15 | 贾冲 | Hydrothermal preparation method of editpotassium cyanide solution |
| CN104909413A (en) * | 2015-06-17 | 2015-09-16 | 中国矿业大学 | Preparation method of ferric oxide nano hexagonal bipyramids |
| CN108314089A (en) * | 2018-02-01 | 2018-07-24 | 济南大学 | A kind of porous flower-shaped α-Fe2O3The synthetic method of self-assembled nanometer material |
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| CN102352134A (en) * | 2011-08-23 | 2012-02-15 | 华南理工大学 | Method for preparing nanometer ferric oxide water-soluble powder |
| CN102352134B (en) * | 2011-08-23 | 2014-04-02 | 华南理工大学 | Method for preparing nanometer ferric oxide water-soluble powder |
| CN102674471A (en) * | 2012-04-16 | 2012-09-19 | 北京航空航天大学 | Preparation method of flower-like mesoporous ferric oxide nano-material |
| CN102826612A (en) * | 2012-09-24 | 2012-12-19 | 厦门大学 | Preparation method of three-dimensional flower-shaped structure alpha-type ferric oxide |
| CN103204550A (en) * | 2013-04-12 | 2013-07-17 | 陕西科技大学 | Controllable preparation method of micron-order Fe2O3 |
| CN103464740A (en) * | 2013-08-16 | 2013-12-25 | 安徽师范大学 | Micro and nano alpha-Fe2O3 material and preparation method thereof |
| CN103464740B (en) * | 2013-08-16 | 2016-06-15 | 安徽师范大学 | A kind of micro-nano α-Fe2O3Material and preparation method thereof |
| CN103771533A (en) * | 2014-01-24 | 2014-05-07 | 天津理工大学 | Preparation method of alpha-Fe2O3 microsphere with flower-like hierarchical structure |
| CN104773743A (en) * | 2015-04-10 | 2015-07-15 | 贾冲 | Hydrothermal preparation method of editpotassium cyanide solution |
| CN104909413A (en) * | 2015-06-17 | 2015-09-16 | 中国矿业大学 | Preparation method of ferric oxide nano hexagonal bipyramids |
| CN108314089A (en) * | 2018-02-01 | 2018-07-24 | 济南大学 | A kind of porous flower-shaped α-Fe2O3The synthetic method of self-assembled nanometer material |
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