CN101538065B - Preparation method of titanium dioxide europium-doped nano-film sol - Google Patents
Preparation method of titanium dioxide europium-doped nano-film sol Download PDFInfo
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- CN101538065B CN101538065B CN2009100478205A CN200910047820A CN101538065B CN 101538065 B CN101538065 B CN 101538065B CN 2009100478205 A CN2009100478205 A CN 2009100478205A CN 200910047820 A CN200910047820 A CN 200910047820A CN 101538065 B CN101538065 B CN 101538065B
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Abstract
The invention discloses a preparation method of titanium dioxide europium-doped nano-film sol. In the method, metatitanic acid (H2TiO3) is washed by distilled water repeatedly, and put into an oven to be baked for 12 hours at 60 DEG C; europium sesquioxide (Eu2O3) is dissolved in nitric acid to obtain europium ion; H2Ti3 and K2CO3 are evenly mixed according to mol ratio of 5.2:1, europium ion is added into the mixture according to 0.2-3% of mass fraction of titanium, and little absolute ethyl alcohol is added into the mixture simultaneously, the mixture being fully ground is put in a muffle to be calcined for 6-15 hours at 600-1000 DEG C, the material being calcined is taken out and added into hydrochloric acid of 1mol/L according to the proportion of 4g/L to be stirred, filtration washing is carried out for 24-72 hours, the filter cake is added into 4-n-butyl ammonium hydroxide or ethylene dimine according to the proportion of 0.4g/L to be stirred for 24-72 hours, is then centrifugated at the high speed centrifugation of 10000r/min to obtain titanium dioxide europium-doped nano-film sol. The invention is convenient in operation, low in cost and suitable for industrialized prosuction.
Description
Technical field
The present invention relates to the preparation of nanometer sheet, is that titanium source, europiumsesquioxide are that the europium source prepares titanium dioxide europium-doped (TiO with the technical grade metatitanic acid specifically
2: Eu
3+) the method for nano-film sol.
Background technology
TiO
2Stable, the indissoluble of chemical property, nontoxic, cost is low, it is causing the researcher extensive interest aspect solar energy converting and storage, the harmful complicated organic matter degradation.It is the ideal photocatalyst, but it is because of forbidden band broad (3.2eV), excite generation electronics one hole right, need near-ultraviolet light (387.5nm). and in solar spectrum, the green light district of light intensity the best part about 500nm, ultraviolet and near ultraviolet part only account for about 5% of total luminous energy, and this causes it very low to the utilization ratio of sunlight, therefore improve and utilize the gordian technique of sun power efficient to be to improve TiO
2Energy gap, the response spectrum of reaction is expanded to visible light, thereby is improved TiO
2The photocatalysis efficiency of nanoparticle.On the other hand, TiO
2The recombination velocity of electric charge carrier be exceedingly fast, have a strong impact on light-catalysed efficient, so expansion TiO
2To photoresonance responding range that absorbs and the recombination rate that reduces current carrier, and adopted TiO
2Nano material is carried out the adulterated improvement of europium, and europium belongs to nontoxic element, can not pollute during application, and the adding of europium has changed TiO
2Condition of surface and crystal field environment, thus the problem of this two aspect solved.Titanium dioxide europium-doped nano-film sol can be made nano film material, and it has all shown wide application prospect in the research of solar cell reflectance coating, electroluminescent display device, reversible photocell and superconducting thin film.
At present, the source of titanium dioxide mainly is the hydrolysis of Butyl Phthalate, and required raw materials cost is higher, and complex process.The nanometer sheet of, even particle size distribution high-purity in order to obtain, anatase octahedrite phase europium doped must manage to take cheap raw material.
Summary of the invention
A kind of titanium dioxide europium-doped (the TiO that provides at the deficiencies in the prior art is provided
2: Eu
3+) preparation method of nano-film sol, this method is simple to operate, and appointed condition is low, and is with low cost, is fit to suitability for industrialized production.
The concrete technical scheme that realizes the object of the invention is:
A kind of preparation method of titanium dioxide europium-doped nano-film sol, this method comprises following concrete steps:
A, with metatitanic acid (H
2TiO
3) distilled water wash repeatedly, put into 60 ℃ baking oven 12 hours. get europiumsesquioxide (Eu
2O
3) in the nitric acid that is dissolved in europium ion;
B, with metatitanic acid (H
2TiO
3) and salt of wormwood (K
2CO
3) be to mix at 5.2: 1 with mol ratio, get the europium ion that makes among a and join in this mixture, and add the dehydrated alcohol of 5ml according to 0.2%～3% of titanium massfraction, fully grind;
C, with gained mixture among the b place retort furnace in 600 ℃～1000 ℃ the reaction 6～15 hours;
Material after d, the taking-up calcining, the hydrochloric acid that adds 1mol/L with the ratio of 4g/L stirred 24～72 hours, behind the filtration washing, filter cake is with the ratio of 0.4g/L, adding 4-n-butyl ammonium hydroxide or quadrol stirred 24～72 hours, centrifugal under the supercentrifuge of 10000r/min then, obtain titanium dioxide europium-doped (TiO
2: Eu
3+) nano-film sol.
The invention has the beneficial effects as follows:
(1), to adopt cheap technical grade metatitanic acid be raw materials for production, operating process is simple when reducing production costs.
(2), 4-n-butyl ammonium hydroxide and quadrol stirred solution can recycle, and reduces the pollution to environment, saves the energy, reduce cost.
(3), gained titanium dioxide europium-doped nano-film vitreosol has good optical property.
Description of drawings
Fig. 1 is the X-ray diffractogram of the titanium dioxide europium-doped powder of embodiment 3 gained
Fig. 2 is the fluorescence spectrum of the titanium dioxide europium-doped powder of embodiment 3 gained
Fig. 3 is the fluorescence spectrum of the titanium dioxide europium-doped colloidal sol of embodiment 3 gained after hydrochloric acid and 4-n-butyl ammonium hydroxide processing
Fig. 4 is the TEM figure of embodiment 3 titanium dioxide europium-doped nano-film sols
Embodiment
Embodiment 1
A, with 5g metatitanic acid (H
2TiO
3) repeatedly use distilled water wash, be put in the baking oven and dried by the fire 12 hours down in 60 ℃, get the europiumsesquioxide (Eu of 0.01g
2O
3) in the nitric acid of the 0.16ml1mol/l that is dissolved in europium ion.
B, with 5g H
2TiO
3With 6.9g K
2CO
3Mixed even, the europium ion of getting among a preparation 0.16ml joins in this mixture, this moment, the quality massfraction that accounts for titanium of europium was 0.2%, added the dehydrated alcohol of 5ml again, fully ground.
C, with mixture among the b place retort furnace in 600 ℃～1000 ℃ the reaction 6 hours.
Material after d, the taking-up calcining, the hydrochloric acid stirring that adds 1mol/L with the ratio of 4g/L, 24 filtration washings as a child, filter cake is with the ratio of 0.4g/L, adding 4-n-butyl ammonium hydroxide stirred 24 hours, under the supercentrifuge of 10000r/min centrifugal 10 minutes then, supernatant liquid was the titanium dioxide europium-doped nano-film vitreosol.
Embodiment 2
A, the 10g metatitanic acid is repeatedly used distilled water wash, be put in the baking oven, get 0.1g europiumsesquioxide (Eu in 60 ℃ of bakings 12 hours down
2O
3) be dissolved in the nitric acid of 1.6ml1mol/l europium ion.
B, with 10g H
2TiO
3With 13.8K
2CO
3Mix, get the 1.6ml europium ion that makes among a and join in this mixture, the massfraction that this moment, europium accounted for titanium is 1%, adds the dehydrated alcohol of 5ml, fully grinds.
C, with mixture among the b place retort furnace in 800 ℃ the reaction 8 hours.
Material after d, the taking-up calcining, the hydrochloric acid stirring that adds 1mol/L with the ratio of 4g/L, 36 filtration washings as a child, filter cake is with the ratio of 0.4g/L, adding quadrol stirred 36 hours, centrifugal under the supercentrifuge of 10000r/min then, obtain supernatant liquid and be corresponding titanium dioxide europium-doped nano-film vitreosol.
Embodiment 3
A, with 10 metatitanic acid (H
2TiO
3) repeatedly use distilled water wash, be put in the baking oven and dried by the fire 12 hours down in 60 ℃, get 0.3g europiumsesquioxide (Eu
2O
3) in the nitric acid of the 4.8ml1mol/l that is dissolved in europium ion.
B, with 10g H
2TiO
3With 13.8gK
2CO
3Mix, get the europium ion 4.8ml that makes among a and add in this mixture, this moment europium account for titanium massfraction 3%, add the dehydrated alcohol of 5ml, fully grind.
C, with mixture among the b place retort furnace in 800 ℃ the reaction 12 hours.
Material after d, the taking-up calcining, the hydrochloric acid stirring that adds 1mol/L with the ratio of 4g/L, 72 filtration washings as a child, filter cake is with the ratio of 0.4g/L, adding 4-n-butyl ammonium hydroxide stirred 72 hours, centrifugal under the supercentrifuge of 10000r/min then, obtain corresponding titanium dioxide europium-doped nano-film vitreosol.
Embodiment 4
A, with 20g metatitanic acid (H
2TiO
3) repeatedly use distilled water wash, be put in the baking oven and dried by the fire 12 hours down in 60 ℃. get the europiumsesquioxide (Eu of 0.4g
2O
3) in the nitric acid that is dissolved in europium ion.
B, with 20g H
2TiO
3With 27.6g K
2CO
3Mix, get in the mixture that the europium ion that makes among a adds, this moment europium account for titanium massfraction 2%, add the 5ml dehydrated alcohol, fully grind.
C, with mixture among the b place retort furnace in 1000 ℃ the reaction 15 hours.
Material after d, the taking-up calcining, the hydrochloric acid stirring that adds 1mol/L with the ratio of 4g/L, 36 filtration washings as a child, the filter cake that obtains is with the ratio of 0.4g/L, adding quadrol stirred 36 hours, centrifugal under the supercentrifuge of 10000r/min then, obtain corresponding titanium dioxide europium-doped nano-film vitreosol.
Embodiment 5
A, with 5g metatitanic acid (H
2TiO
3) repeatedly use distilled water wash, be put in the baking oven and dried by the fire 12 hours down in 60 ℃. get 0.05g europiumsesquioxide (Eu
2O
3) in the nitric acid of the 0.80ml1mol/l that is dissolved in europium ion.
B, with 5g H
2TiO
3With 6.9g K
2CO
3Mix, get in the mixture that the europium ion that makes among a adds, this moment europium account for titanium massfraction 1%, add the 5ml dehydrated alcohol, fully grind.
C, with mixture among the b place retort furnace in 600 ℃ the reaction 10 hours.
Material after d, the taking-up calcining, the hydrochloric acid stirring that adds 1mol/L with the ratio of 4g/L, 48 filtration washings as a child, filter cake is with the ratio of 0.4g/L, adding 4-n-butyl ammonium hydroxide stirred 48 hours, centrifugal under the supercentrifuge of 10000r/min then, obtain corresponding titanium dioxide europium-doped nano-film vitreosol.
Embodiment 6
A, with 20 metatitanic acid (H
2TiO
3) repeatedly use distilled water wash, be put in the baking oven and dried by the fire 12 hours down in 60 ℃, get the europiumsesquioxide (Eu of 0.08g
2O
3) in the nitric acid of the 1.28ml 1mol/l that is dissolved in europium ion.
B, with 20g H
2TiO
3With 27.6gK
2CO
3Mix, get in the mixture that the europium ion that makes among a adds, this moment europium account for titanium massfraction 0.4%, and add the 5ml dehydrated alcohol, fully grind.
C, with mixture among the b place retort furnace in 700 ℃ the reaction 14 hours.
Material after d, the taking-up calcining, the hydrochloric acid stirring that adds 1mol/L with the ratio of 4g/L, 56 filtration washings as a child, the filter cake that obtains is with the ratio of 0.4g/L, adding quadrol stirred 56 hours, centrifugal under the supercentrifuge of 10000r/min then, obtain corresponding titanium dioxide europium-doped nano-film vitreosol.
Claims (1)
1. the preparation method of a titanium dioxide europium-doped nano-film sol is characterized in that it comprises following concrete steps:
A, with metatitanic acid (H
2TiO
3) distilled water wash repeatedly, put into 60 ℃ baking oven 12 hours, get europiumsesquioxide (Eu
2O
3) be dissolved in the nitric acid europium ion;
B, with metatitanic acid (H
2TiO
3) and salt of wormwood (K
2CO
3) be to mix at 5.2: 1 with mol ratio, get the europium ion that makes among a and join in this mixture, and add the dehydrated alcohol of 5ml according to 0.2%～3% of titanium massfraction, fully grind;
C, with gained mixture among the b place retort furnace in 600 ℃～1000 ℃ the calcining 6～15 hours;
Material after d, the taking-up calcining, the hydrochloric acid that adds 1mol/L with the ratio of 4g/L stirred 24～72 hours, behind the filtration washing, filter cake is with the ratio of 0.4g/L, adding 4-n-butyl ammonium hydroxide or quadrol stirred 24～72 hours, centrifugal under the supercentrifuge of 10000r/min then, obtain titanium dioxide europium-doped TiO
2: Eu
3+Nano-film sol.
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| CN108380199B (en) * | 2018-03-16 | 2020-09-01 | 沈阳理工大学 | Method for preparing europium-titanium composite nano oxide powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631521A (en) * | 2004-11-06 | 2005-06-29 | 重庆工学院 | Process for preparing highly efficient titania photocatalyst |
| CN1769184A (en) * | 2005-09-27 | 2006-05-10 | 广东省生态环境与土壤研究所 | Method for preparing high activity titanium dioxide sol using industrial metatitanic acid as material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631521A (en) * | 2004-11-06 | 2005-06-29 | 重庆工学院 | Process for preparing highly efficient titania photocatalyst |
| CN1769184A (en) * | 2005-09-27 | 2006-05-10 | 广东省生态环境与土壤研究所 | Method for preparing high activity titanium dioxide sol using industrial metatitanic acid as material |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2005-330133A 2005.12.02 |
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Inventor after: Li Qiang Inventor after: Chu Jing Inventor after: Song Jie Inventor after: Li Caixia Inventor after: Zhang Na Inventor before: Li Qiang Inventor before: Chu Jing Inventor before: Song Jie Inventor before: Li Caixia Inventor before: Zhang Na |
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