CN103788945A - Preparation method of rare earth luminescence mesoporous titania hybrid material - Google Patents
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- CN103788945A CN103788945A CN201410011570.0A CN201410011570A CN103788945A CN 103788945 A CN103788945 A CN 103788945A CN 201410011570 A CN201410011570 A CN 201410011570A CN 103788945 A CN103788945 A CN 103788945A
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Abstract
The invention discloses a preparation method of a rare earth luminescence mesoporous titania hybrid material. The preparation method mainly comprises the following steps: firstly, synthesizing an ordered mesoporous titania material and modifying the mesoporous titania through 2,2'-dipyridyl-4,4'-dicarboxylic acid; then enabling the modified ordered mesoporous titania and synthesized binary rare earth complexes to carry out reflux reaction for hours in ethyl alcohol and obtain a solid product; and washing and drying to prepare a rare earth luminescence mesoporous titania hybrid material. Through the preparation method of the rare earth luminescence mesoporous titania hybrid material, the rare earth complexes are grafted to an ordered mesoporous titania matrix through a covalent bond; the prepared rare earth luminescence mesoporous titania hybrid material is capable of obtaining visual and near-infrared light emission under visible light excitation; and the rare earth luminescence mesoporous titania hybrid material shows potential application prospects in solar cells and biological materials.
Description
Technical field
The invention belongs to the multi-functional mesoporous technical field of material of rare earth, be specifically related to a kind of preparation method of rare earth luminous mesoporous TiO 2 hybrid material.
Background technology
Ordered mesoporous titanium dioxide, because of characteristics such as its porous and high-specific surface areas, shows wide application prospect at aspects such as solar cell, water pollution control, photochemical catalysis.Mesoporous TiO 2 has higher catalytic activity as important photocatalyst than nanoparticle titanium dioxide, and the high-specific surface area of its order mesoporous structure has increased its adsorptive power, can be used as the carrier that drug release and organism transmit, aspect chemical sensor, luminescent material and nano material microreactor, be expected to the effect that performance is larger.
Rare earth organic complex, as efficient luminophore, is early familiar with by people, but its chemical stability and mechanical stability have limited its application in actual production and life.Facts have proved rare earth compounding is incorporated in the middle of mesoporous matrix, can improve the stability of its light and heat simultaneously, and avoided the impact of external environment, thereby effectively improved its luminescent properties.The research that at present rare earth compounding is incorporated into silicon and is mesoporous material is a lot, is that the report of mesoporous material research is relatively less and mix non-silicon for it.Mesoporous TiO 2 is transition metal oxide mesoporous material as the non-silicon of one, and the meso-hole structure of its high-sequential becomes one of ideal carrier loading rare earth compounding.If the grafting of rare earth compounding covalency, in ordered mesoporous titanium dioxide material, is obtained to rare earth ordered mesoporous titanium dioxide luminescent material, is expected to be more widely used in biologic applications and area of solar cell.
Summary of the invention
For above-mentioned problem, one of the object of the invention is to provide rare earth luminous mesoporous TiO 2 hybrid material.
Two of object of the present invention is to provide the preparation method of this rare earth luminous mesoporous TiO 2 hybrid material.
For achieving the above object, technical scheme provided by the present invention is:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1～3ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 20～24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation, in alcohol solvent, reflux and remove template, obtain ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is placed in N, in N '-solvent dimethylformamide, return stirring 3～5h, after filtering solid product, wash, obtain 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add the chlorate of rare earth metal, at 70～90 ℃, reflux 4～5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, use deionized water and washing with alcohol three times, after being dried, obtain binary rare-earth title complex;
(4) by 2,2 '-dipyridyl-4, binary rare-earth title complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and step 3 adds in 10 ~ 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain rare earth luminous mesoporous TiO 2 hybrid material.
The described gel product of step in the present invention (1) is adding after ammoniacal liquor container sealing, and room temperature leaves standstill 24 hours.
Described in step in the present invention (2) 2,2 '-dipyridyl-4, the mol ratio of 4 '-dicarboxylic acid and ordered mesoporous titanium dioxide material is (0.5～1): 1.
The described rare earth metal in step in the present invention (3) or (4) is the one in europium, samarium, ytterbium, neodymium, erbium, holmium, thulium.
The chlorate of step in the present invention (3) rare earth metal and the mol ratio of thiophene trifluoroacetylacetone are 1:3.
Described in step in the present invention (4) 2,2 '-dipyridyl-4, the quality of the mesoporous TiO 2 that 4 '-dicarboxylic acid is modified is 0.08～0.1g, the mole number of binary rare-earth title complex is 0.5mmol.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the luminous mesoporous TiO 2 hybrid material of europium that makes of the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope figure of the luminous mesoporous TiO 2 hybrid material of europium that makes of the embodiment of the present invention 1.
Fig. 3 is the fluorescence spectrum of the luminous mesoporous TiO 2 hybrid material of samarium that makes of the embodiment of the present invention 2.
Embodiment
In the following examples, the invention will be further elaborated, but the invention is not restricted to this.
Embodiment 1:
The present embodiment provides a kind of rare earth luminous mesoporous TiO 2 hybrid material, and its preparation comprises the following steps:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1.26ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor container sealing, room temperature leaves standstill 24 hours, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation refluxes and removes template in alcohol solvent, obtains ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is pressed (0.5～1): 1 mol ratio is placed in N, in N '-solvent dimethylformamide, return stirring 5h, after solid product is filtered, washed, obtains 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add Europium trichloride, the mol ratio of Europium trichloride and thiophene trifluoroacetylacetone is 1:3, at 80 ℃, reflux 5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, wash respectively three times with deionized water and ethanol, obtain binary europium complex after dry;
(4) by 0.08～0.1g 2,2 '-dipyridyl-4, binary europium complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and 0.5mmol adds in 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain the luminous mesoporous TiO 2 hybrid material of europium.
Embodiment 2:
The present embodiment provides a kind of preparation method of rare earth luminous mesoporous TiO 2 hybrid material, and its basic step is identical with embodiment 1, and its difference is its following concrete steps difference:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1.26ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor container sealing, room temperature leaves standstill 24 hours, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation refluxes and removes template in alcohol solvent, obtains ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is pressed (0.5～1): 1 mol ratio is placed in N, in N '-solvent dimethylformamide, return stirring 5h, after solid product is filtered, washed, obtains 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add samarium trichloride, the mol ratio of samarium trichloride and thiophene trifluoroacetylacetone is 1:3, at 80 ℃, reflux 5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, wash respectively three times with deionized water and ethanol, obtain binary samarium complex after dry;
(4) by 0.08～0.1g 2,2 '-dipyridyl-4, binary samarium complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and 0.5mmol adds in 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain the luminous mesoporous TiO 2 hybrid material of samarium.
Embodiment 3:
The present embodiment provides a kind of preparation method of rare earth luminous mesoporous TiO 2 hybrid material, and its basic step is identical with embodiment 1, and its difference is its following concrete steps difference:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1.26ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor container sealing, room temperature leaves standstill 24 hours, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation refluxes and removes template in alcohol solvent, obtains ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is pressed (0.5～1): 1 mol ratio is placed in N, in N '-solvent dimethylformamide, return stirring 5h, after solid product is filtered, washed, obtains 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add Ytterbium trichloride, the mol ratio of Ytterbium trichloride and thiophene trifluoroacetylacetone is 1:3, at 80 ℃, reflux 5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, wash respectively three times with deionized water and ethanol, obtain binary ytterbium complex after dry;
(4) by 0.08～0.1g 2,2 '-dipyridyl-4, binary ytterbium complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and 0.5mmol adds in 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain the luminous mesoporous TiO 2 hybrid material of ytterbium.
Embodiment 4:
The present embodiment provides a kind of preparation method of rare earth luminous mesoporous TiO 2 hybrid material, and its basic step is identical with embodiment 1, and its difference is its following concrete steps difference:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1.26ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor container sealing, room temperature leaves standstill 24 hours, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation refluxes and removes template in alcohol solvent, obtains ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is pressed (0.5～1): 1 mol ratio is placed in N, in N '-solvent dimethylformamide, return stirring 5h, after solid product is filtered, washed, obtains 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add Neodymium trichloride, the mol ratio of Neodymium trichloride and thiophene trifluoroacetylacetone is 1:3, at 80 ℃, reflux 5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, wash respectively three times with deionized water and ethanol, obtain binary neodymium title complex after dry;
(4) by 0.08～0.1g 2,2 '-dipyridyl-4, binary neodymium title complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and 0.5mmol adds in 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain the luminous mesoporous TiO 2 hybrid material of neodymium.
Embodiment 5:
The present embodiment provides a kind of preparation method of rare earth luminous mesoporous TiO 2 hybrid material, and its basic step is identical with embodiment 1, and its difference is its following concrete steps difference:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1.26ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor container sealing, room temperature leaves standstill 24 hours, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation refluxes and removes template in alcohol solvent, obtains ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is pressed (0.5～1): 1 mol ratio is placed in N, in N '-solvent dimethylformamide, return stirring 5h, after solid product is filtered, washed, obtains 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add Erbium trichloride, the mol ratio of Erbium trichloride and thiophene trifluoroacetylacetone is 1:3, at 80 ℃, reflux 5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, wash respectively three times with deionized water and ethanol, obtain binary erbium title complex after dry;
(4) by 0.08～0.1g 2,2 '-dipyridyl-4, binary erbium title complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and 0.5mmol adds in 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain the luminous mesoporous TiO 2 hybrid material of erbium.
Embodiment 6:
The present embodiment provides a kind of preparation method of rare earth luminous mesoporous TiO 2 hybrid material, and its basic step is identical with embodiment 1, and its difference is its following concrete steps difference:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1.26ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor container sealing, room temperature leaves standstill 24 hours, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation refluxes and removes template in alcohol solvent, obtains ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is pressed (0.5～1): 1 mol ratio is placed in N, in N '-solvent dimethylformamide, return stirring 5h, after solid product is filtered, washed, obtains 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add Holmium trichloride, the mol ratio of Holmium trichloride and thiophene trifluoroacetylacetone is 1:3, at 80 ℃, reflux 5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, wash respectively three times with deionized water and ethanol, obtain binary holmium title complex after dry;
(4) by 0.08～0.1g 2,2 '-dipyridyl-4, binary holmium title complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and 0.5mmol adds in 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain the luminous mesoporous TiO 2 hybrid material of holmium.
Embodiment 7:
The present embodiment provides a kind of preparation method of rare earth luminous mesoporous TiO 2 hybrid material, and its basic step is identical with embodiment 1, and its difference is its following concrete steps difference:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1.26ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor container sealing, room temperature leaves standstill 24 hours, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation refluxes and removes template in alcohol solvent, obtains ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is pressed (0.5～1): 1 mol ratio is placed in N, in N '-solvent dimethylformamide, return stirring 5h, after solid product is filtered, washed, obtains 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add thulium chloride, the mol ratio of thulium chloride and thiophene trifluoroacetylacetone is 1:3, at 80 ℃, reflux 5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, wash respectively three times with deionized water and ethanol, obtain binary thulium title complex after dry;
(4) by 0.08～0.1g 2,2 '-dipyridyl-4, binary thulium title complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and 0.5mmol adds in 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain the luminous mesoporous TiO 2 hybrid material of thulium.
Can find out by Fig. 1 to Fig. 3:
Fig. 1 is the infrared spectrogram of the luminous mesoporous TiO 2 hybrid material of europium that makes of the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope figure of the luminous mesoporous TiO 2 hybrid material of europium that makes of the embodiment of the present invention 1, the mesopore orbit that can find out this hybridization mesoporous material still keeps good order after grafting europium complex, presents two-dimentional hexagonal mesoporous structure.
Fig. 3 is the excitation and emission spectra figure of the luminous mesoporous TiO 2 hybrid material of samarium that makes of the embodiment of the present invention 2, with Sm
3+the strongest emission wavelength of 951nm for monitoring wavelength, obtain the excitation spectrum (the left figure of Fig. 3) of this material, selecting 401nm visible region wavelength is excitation wavelength, obtaining this material has near infrared emission at 800-1700 nm, wherein the strongest emission peak is positioned at 951nm.
The present invention is take ordered mesoporous titanium dioxide as matrix, by covalent linkage by rare earth compounding grafting in the mesopore orbit of mesoporous TiO 2, prepare thus a class novel rare-earth organic and inorganic mesoporous titanium dioxide hybrid luminescent materials.The rare earth luminous mesoporous TiO 2 hybrid material of gained has good fluorescence property and thermostability, and has kept the hexagonal mesoporous pore passage structure of two dimension of mesoporous TiO 2, is expected to advance its application aspect photochemical catalysis, stored energy conversion and sensor.
Be only better possible embodiments of the present invention to above-described embodiment, not in order to limit to the scope of the claims of the present invention, the same as the previously described embodiments or similar method of described employing all should be within protection scope of the present invention.
Claims (6)
1. the preparation method of rare earth luminous mesoporous TiO 2 hybrid material, is characterized in that, the method has following step of preparation process:
(1) taking 1g P123 is dissolved in 20g ethanol, under fully stirring, successively add respectively the HCl solution of 1～3ml 6mol/L and the titanium tetraisopropylate of 1.5～2ml, 25 ℃ of constant temperature stir 20～24h, revolve and evaporate unnecessary ethanolic soln with Rotary Evaporators afterwards, be placed in 40 ℃ of oven for drying gels, gel product is adding after ammoniacal liquor, produce white precipitate, by white precipitate 65 ℃ of oven dry, collecting precipitation, in alcohol solvent, reflux and remove template, obtain ordered mesoporous titanium dioxide;
(2) by 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide of 4 '-dicarboxylic acid and preparation is placed in N, in N '-solvent dimethylformamide, return stirring 3～5h, after filtering solid product, wash, obtain 2,2 '-dipyridyl-4, the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified;
(3) thiophene trifluoroacetylacetone is dissolved in ethanol, splash into the NaOH solution of 1mol/L, regulate pH value to 6～8, dropwise add the chlorate of rare earth metal, at 70～90 ℃, reflux 4～5 hours, to be cooled to room temperature, add deionized water that solid reactant is separated out, after filtering, use deionized water and washing with alcohol three times, after being dried, obtain binary rare-earth title complex;
(4) by 2,2 '-dipyridyl-4, binary rare-earth title complex prepared by the ordered mesoporous titanium dioxide that 4 '-dicarboxylic acid is modified and step 3 adds in 10 ~ 20mL ethanol, reflux 4 hours, solid product is filtered, washed, obtain rare earth luminous mesoporous TiO 2 hybrid material.
2. the preparation method of rare earth luminous mesoporous TiO 2 hybrid material according to claim 1, is characterized in that the described gel product of step (1) is adding after ammoniacal liquor container sealing, and room temperature leaves standstill 24 hours.
3. the preparation method of rare earth luminous mesoporous TiO 2 hybrid material according to claim 1, it is characterized in that step (2) described 2,2 '-dipyridyl-4, the mol ratio of 4 '-dicarboxylic acid and ordered mesoporous titanium dioxide material is 0.5～1:1.
4. the preparation method of rare earth luminous mesoporous TiO 2 hybrid material according to claim 1, is characterized in that the described rare earth metal in step (3) or (4) is the one in europium, samarium, ytterbium, neodymium, erbium, holmium, thulium.
5. the preparation method of rare earth luminous mesoporous TiO 2 hybrid material according to claim 1, is characterized in that step (3) the described chlorate of rare earth metal and the mol ratio of thiophene trifluoroacetylacetone are 1:3.
6. the preparation method of rare earth luminous mesoporous TiO 2 hybrid material according to claim 1, it is characterized in that step (4) described 2,2 '-dipyridyl-4, the quality of the mesoporous TiO 2 that 4 '-dicarboxylic acid is modified is 0.08～0.1g, and the mole number of binary rare-earth title complex is 0.5mmol.
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| CN107384375A (en) * | 2017-07-21 | 2017-11-24 | 洛阳师范学院 | A kind of rare earth luminous silicon dioxide hybrid materials and its preparation method and application |
| CN109294553A (en) * | 2018-11-28 | 2019-02-01 | 青岛大学 | A kind of titania additive rare-earth complex composite material and preparation method |
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| CN109294553A (en) * | 2018-11-28 | 2019-02-01 | 青岛大学 | A kind of titania additive rare-earth complex composite material and preparation method |
| CN109294553B (en) * | 2018-11-28 | 2021-08-13 | 青岛大学 | Titanium dioxide doped rare earth complex composite material and preparation method thereof |
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Application publication date: 20140514 |