CN103041813A - Preparation method of titanium dioxide coated iron trioxide hollow sphere - Google Patents
Preparation method of titanium dioxide coated iron trioxide hollow sphere Download PDFInfo
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- CN103041813A CN103041813A CN2012105250165A CN201210525016A CN103041813A CN 103041813 A CN103041813 A CN 103041813A CN 2012105250165 A CN2012105250165 A CN 2012105250165A CN 201210525016 A CN201210525016 A CN 201210525016A CN 103041813 A CN103041813 A CN 103041813A
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- titanium dioxide
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Abstract
The invention discloses a preparation method of a titanium dioxide coated iron trioxide hollow sphere. The preparation method comprises the following steps: using a carbon sphere as a template and synthesizing iron trioxide at lower temperature by using perchloride iron as an iron source; and then, using tetrabutyl titanate as a titanium source to synthesize the iron trioxide hollow sphere. The method provided by the invention is simple and mild and low in reaction temperature, and the thickness of a titanium dioxide coating can be adjusted by changing the addition of tetrabutyl titanate.
Description
Technical field
The present invention relates to the inorganic semiconductor composite, that concrete is a kind of preparation method of coated by titanium dioxide di-iron trioxide hollow ball.
Background technology
Because nano-TiO
2Have good chemical stability, abrasion resistance, low cost and can directly utilize the advantage such as sunshine, and have broad application prospects at aspects such as opto-electronic conversion, chemical synthesis and photochemical catalytic oxidation environmental contaminants, but because TiO
2Photochemical catalyst greater band gap (Eg=3.2 eV, λ=387 nm), ultraviolet ray excited lower at λ＜387 nm only, the valence band electronics just can transit to and form light induced electron and hole on the conduction band, and, because the electronics that optical excitation produces and hole is compound, cause photo-quantum efficiency very low, for overcoming these shortcomings, people take multiple means to TiO improving its visible light catalysis activity and catalytic efficiency, effectively utilizing the aspect such as solar energy to carry out a large amount of further investigations
2Carry out modification, make TiO
2Response spectrum expand to visible light, and the establishment electron-hole is compound, improves nano-TiO
2Photocatalysis efficiency.
Doped transition metal ions can be at TiO
2Introduce defective locations in the lattice or change degree of crystallinity, thereby affect the compound of electronics and hole, the while may form doped energy-band and expand the scope of light absorption wavelength, Fe
2O
3As a kind of semi-conducting material, have narrower energy gap (Eg=2.2 eV, λ=563 nm), its absorption spectrum and solar spectral comparatively mate, and can directly utilize solar energy; But, Fe
2O
3The life-span in hole is short, and photoetch easily occurs, therefore with Fe
2O
3And TiO
2Advantage combines, and uses Fe
3+Perhaps Fe
2O
3Modification TiO
2Become study hotspot in recent years.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of coated by titanium dioxide di-iron trioxide hollow ball, can regulate the thickness of coated by titanium dioxide layer by the addition that changes butyl titanate, the coated by titanium dioxide di-iron trioxide hollow ball size uniform that this method is prepared, diameter is at 850 ~ 1100 nm, and the shell thickness of coated by titanium dioxide is between 50 ~ 100 nm.
The preparation method of coated by titanium dioxide di-iron trioxide hollow ball provided by the present invention, concrete, may further comprise the steps:
(1) glucose is dissolved in the deionized water, forming mass concentration is the solution of 0.15 ~ 0.20 g/mL, this solution is moved in the reactor carry out hydro-thermal reaction, and temperature is 160 ~ 180 ℃, and the reaction time is 6 ~ 8 h, and centrifugal drying obtains the carbon ball template;
(2) ferric sesquichloride is dissolved in the mixed solution of absolute ethyl alcohol and deionized water, wherein the volume ratio of absolute ethyl alcohol and deionized water is 6:1, and the concentration of iron ion is 0.05 ~ 0.1 mol/L;
(3) urea is dissolved in the mentioned solution, is stirred to dissolving, wherein the mol ratio of urea and iron ion is 10:1;
(4) the carbon ball template of step (1) gained is added in the solution of step (3) gained, the mol ratio of carbon ball and iron ion is 8:1, transfers in the baking oven 60 ~ 80 ℃ after mixing and is incubated 48 hours, centrifugal drying;
(5) with the sample dissolution of step (4) gained in the mixed solution of absolute ethyl alcohol and deionized water, wherein the volume ratio of absolute ethyl alcohol and deionized water is 6:1, butyl titanate is added in the mentioned solution, stir, wherein the mol ratio of titanium ion and iron ion is 1:1 ~ 1:2;
(6) with the sample of step (5) gained 450 ~ 500 ℃ of roastings 2 hours, obtain coated by titanium dioxide di-iron trioxide hollow ball.
Description of drawings
Fig. 1 is the TEM figure of the prepared di-iron trioxide hollow ball of embodiment 1.
Fig. 2 is the XRD figure of the prepared coated by titanium dioxide di-iron trioxide hollow ball of embodiment 2, and sign * is the characteristic peak of titanium dioxide among the figure, is the characteristic peak of di-iron trioxide.
Fig. 3 is the TEM figure of the prepared coated by titanium dioxide di-iron trioxide hollow ball of embodiment 2.
Fig. 4 is the TEM figure of the prepared coated by titanium dioxide di-iron trioxide hollow ball of embodiment 3.
The specific embodiment
Below further describe the present invention by the specific embodiment, as known by the technical knowledge, the present invention also can describe by other the scheme that does not break away from the technology of the present invention feature, thus all within the scope of the present invention or the change that is equal in the scope of the invention all be included in the invention.
Embodiment 1
6 g glucose are dissolved in the 40 mL deionized waters, and forming mass concentration is the solution of 0.15 g/mL, this solution is moved in the reactor carry out hydro-thermal reaction, and temperature is 180 ℃, and the reaction time is 6 h, and centrifugal drying obtains the carbon ball template; 0.82 g ferric sesquichloride is dissolved in the mixed solution of 56 mL absolute ethyl alcohols and deionized water, wherein the volume ratio of absolute ethyl alcohol and deionized water is 6:1,1.8 g urea are dissolved in the mentioned solution, be stirred to dissolving, 0.3 g carbon ball template is added in the mentioned solution, transfer in the baking oven 60 ℃ of insulations 48 hours after mixing, centrifugal drying.The sample of gained was removed the carbon ball template in 2 hours 450 ℃ of roastings, obtained Fe
2O
3Hollow ball is to present embodiment product (Fe
2O
3Hollow ball) carry out transmission electron microscope observing its microscopic appearance, the result as shown in Figure 1, prepared Fe
2O
3Sample is size uniform, the hollow ball shape structure of diameter about 800 ~ 1000 nm.
8 g glucose are dissolved in the 40 mL deionized waters, and forming mass concentration is the solution of 0.2 g/mL, this solution is moved in the reactor carry out hydro-thermal reaction, and temperature is 160 ℃, and the reaction time is 8 h, and centrifugal drying obtains the carbon ball template; 0.82 g ferric sesquichloride is dissolved in the mixed solution of 56 mL absolute ethyl alcohols and deionized water, wherein the volume ratio of absolute ethyl alcohol and deionized water is 6:1,1.8 g urea are dissolved in the mentioned solution, be stirred to dissolving, 0.3 g carbon ball template is added in the mentioned solution, transfer in the baking oven 60 ℃ of insulations 48 hours after mixing, centrifugal drying, the sample of gained was removed the carbon ball template in 2 hours 500 ℃ of roastings, obtained Fe
2O
3Hollow ball, size is similar to the result of embodiment 1 gained to structure.
Embodiment 3
In the mixed solution of 56 mL absolute ethyl alcohols and deionized water, wherein the volume ratio of absolute ethyl alcohol and deionized water is 6:1 with the sample dispersion of not heat-treating prepared among the 0.48 g embodiment 1; The butyl titanate of 0.35 mL is added in the mentioned solution, the mol ratio that makes titanium ion and iron ion is 1:2, stir, with solution in baking oven 60 ℃ the insulation 48 hours, centrifugal drying, the sample of gained was 450 ℃ of roastings 2 hours, obtain coated by titanium dioxide di-iron trioxide hollow ball, present embodiment product (coated by titanium dioxide di-iron trioxide hollow ball) is carried out X-ray powder diffraction result as shown in Figure 2, sign * is the characteristic peak of titanium dioxide among the figure, be the characteristic peak of di-iron trioxide, Fe appears in prepared sample simultaneously
2O
3And TiO
2Characteristic peak, and consistent with standard P DF card, product is Fe
2O
3And TiO
2Composite construction, product is carried out transmission electron microscope observing its microscopic appearance, the result as shown in Figure 3, product is nuclear-shell hollow-core construction, and the thickness of coated by titanium dioxide layer is about about 50 nm.
Embodiment 4
In the mixed solution of 56 mL absolute ethyl alcohols and deionized water, wherein the volume ratio of absolute ethyl alcohol and deionized water is 6:1 with the sample dispersion of not heat-treating prepared among the 0.48 g embodiment 2; The butyl titanate of 0.7 mL is added in the mentioned solution, the mol ratio that makes titanium ion and iron ion is 1:1, stir, with solution in baking oven 60 ℃ the insulation 48 hours, centrifugal drying, the sample of gained was 450 ℃ of roastings 2 hours, obtain coated by titanium dioxide di-iron trioxide hollow ball, present embodiment product (coated by titanium dioxide di-iron trioxide hollow ball) is carried out transmission electron microscope to observe its microscopic appearance, the result as shown in Figure 4, product is nuclear-shell hollow ball structure, and the thickness of coated by titanium dioxide layer is about about 100 nm.
Claims (4)
1. the preparation method of a coated by titanium dioxide di-iron trioxide hollow ball is characterized in that may further comprise the steps:
(1) preparation carbon ball template;
(2) ferric sesquichloride is dissolved in the mixed solution of absolute ethyl alcohol and deionized water, the concentration of iron ion is 0.05 ~ 0.1 mol/L;
(3) urea is dissolved in the mentioned solution, is stirred to dissolving, wherein the mol ratio of urea and iron ion is 10:1;
(4) the carbon ball template of step (1) gained is added in the solution of step (3) gained, the mol ratio of carbon ball and iron ion is 8:1, transfers in the baking oven 60 ~ 80 ℃ after mixing and is incubated 48 hours, centrifugal drying;
(5) with the sample dissolution of step (4) gained in the mixed solution of absolute ethyl alcohol and deionized water, butyl titanate is added in the mentioned solution, stir, wherein the mol ratio of titanium ion and iron ion is 1:1 ~ 1:2;
(6) with the sample of step (5) gained 450 ~ 500 ℃ of roastings 2 hours, obtain coated by titanium dioxide di-iron trioxide hollow ball.
2. the preparation method of a kind of coated by titanium dioxide di-iron trioxide hollow ball as claimed in claim 1, it is characterized in that: the step of described preparation carbon ball template is: glucose is dissolved in the deionized water, forming mass concentration is the solution of 0.15 ~ 0.20 g/mL, to carry out hydro-thermal reaction in this solution immigration reactor, temperature is 160 ~ 180 ℃, reaction time is 6 ~ 8 h, and centrifugal drying obtains the carbon ball template.
3. the preparation method of a kind of coated by titanium dioxide di-iron trioxide hollow ball as claimed in claim 1, it is characterized in that: the volume ratio of described absolute ethyl alcohol and deionized water is 6:1.
4. the preparation method of a kind of coated by titanium dioxide di-iron trioxide hollow ball as claimed in claim 1, it is characterized in that: described coated by titanium dioxide di-iron trioxide hollow ball size uniform, diameter is at 850 ~ 1100 nm, and the shell thickness of coated by titanium dioxide is between 50 ~ 100 nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108816212A (en) * | 2018-07-10 | 2018-11-16 | 中国计量大学 | A kind of preparation method of optically catalytic TiO 2 composite material |
| CN110624548A (en) * | 2019-09-26 | 2019-12-31 | 中国矿业大学(北京) | Preparation method of multistage iron oxide catalyst for removing heteroatoms in coal liquefied oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628236A (en) * | 2009-08-03 | 2010-01-20 | 浙江理工大学 | Preparation method of kieselguhr load type compound photocatalyst with iron ions doped titanium dioxide |
| CN101890350A (en) * | 2010-07-21 | 2010-11-24 | 江苏大学 | Method for preparing Fe3+doped TiO2 hollow sphere catalyst and application thereof |
-
2012
- 2012-12-10 CN CN2012105250165A patent/CN103041813A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628236A (en) * | 2009-08-03 | 2010-01-20 | 浙江理工大学 | Preparation method of kieselguhr load type compound photocatalyst with iron ions doped titanium dioxide |
| CN101890350A (en) * | 2010-07-21 | 2010-11-24 | 江苏大学 | Method for preparing Fe3+doped TiO2 hollow sphere catalyst and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 龚潇等: "TiO2/α-Fe2O3复合光催化剂的制备及表征", 《硅酸盐学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108816212A (en) * | 2018-07-10 | 2018-11-16 | 中国计量大学 | A kind of preparation method of optically catalytic TiO 2 composite material |
| CN110624548A (en) * | 2019-09-26 | 2019-12-31 | 中国矿业大学(北京) | Preparation method of multistage iron oxide catalyst for removing heteroatoms in coal liquefied oil |
| CN110624548B (en) * | 2019-09-26 | 2020-09-08 | 中国矿业大学(北京) | Preparation method of multistage iron oxide catalyst for removing heteroatoms in coal liquefied oil |
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Application publication date: 20130417 |