CN103599770A - Preparation method of TiO2/InVO4 nanojunction composite material - Google Patents
Preparation method of TiO2/InVO4 nanojunction composite material Download PDFInfo
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- CN103599770A CN103599770A CN201310585798.6A CN201310585798A CN103599770A CN 103599770 A CN103599770 A CN 103599770A CN 201310585798 A CN201310585798 A CN 201310585798A CN 103599770 A CN103599770 A CN 103599770A
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Abstract
The invention relates to the field of semiconductor materials, and aims to provide a preparation method of a TiO2/InVO4 nanojunction composite material. The preparation method comprises the following steps of: adding InVO4 particles to a polymer type TiO2 sol, and after reacting, filtering and washing the precipitate to obtain powder; retaining the heat of the powder in a muffle furnace for 2h to obtain TiO2 quantum dot modified InVO4 particles; dispersing the modified InVO4 particles in ethanol water to obtain a system, adding the mixed solution of butyl titanate and absolute ethyl alcohol to the system under the condition of stirring in a water bath, and then filtering, washing and drying the precipitate to obtain the TiO2/InVO4 nanojunction composite material. The preparation method of the TiO2/InVO4 nanojunction composite material has the characteristics that the forming of core-shell structures caused by excessive coating or homogeneous precipitation of nanocrystals in solution is avoided and the normal-pressure liquid phase growth problem of the nanocrystals is solved by taking hydrated titanium ions as growth units; the surface of the prepared nanojunction composite material shows photocatalytic oxidation and reduction properties simultaneously.
Description
Technical field
The invention relates to field of semiconductor materials, particularly TiO
2/ InVO
4the preparation method of nano junction composite.
Background technology
TiO
2be a kind of important function semi-conducting material, in fields such as the energy, environment, electronic information, have broad application prospects.Yet lower quantum efficiency has limited its practical application, expand photoresponse wavelength, promote photo-generated carrier separated, improve material quantum efficiency is TiO always
2the important directions of research.Utilize narrow gap semiconductor, as CdS, WS
2, ZnFe
2o
4, InVO
4deng, with TiO
2compound one side can be effectively by TiO
2photoresponse wavelength be extended to visible light wave range, can also promote on the other hand the migration of light induced electron between different semi-conducting materials with separated, reduce the compound of light induced electron, hole, improve quantum efficiency.
Along with the development of nanometer technology, increasing research starts to lay particular emphasis on the design by low dimensional structures, promotes traditional material performance or gives its new characteristic.By structure nano junction composite construction, contribute on same surface, to form the two-phase microcell with oxidisability and reproducibility, become the important channel of design novel photocatalysis semi-conducting material.TiO
2/ InVO
4composite is a kind of emerging composite semiconductor system, yet current its preparation or be a kind of simple physical mixed sintering causes photocatalysis efficiency not high; Be the coated nucleocapsid structure that forms of chemistry, only have a kind of semiconductor to be positioned at surface, cause selective to photochemical catalytic oxidation or reduction.Therefore by structure nano junction composite construction, prepare novel TiO
2/ InVO
4composite, has broad application prospects.
Summary of the invention
Main purpose of the present invention is to overcome deficiency of the prior art, and preparation TiO is provided
2/ InVO
4the method of nano junction composite.For solving the problems of the technologies described above, solution of the present invention is:
TiO is provided
2/ InVO
4the preparation method of nano junction composite, comprises the following steps:
Steps A: by InVO
4it is 1%～5% polymer-type TiO that particle joins solid content
2in colloidal sol, and to make the mol ratio of In and Ti be 1: 50～1: 10, then after 50 ℃ of stirring in water bath 1h～10h, by sedimentation and filtration, obtain powders by least 3 post-dryings of absolute ethanol washing, this powder is placed in to 350 ℃ of insulation 2h of Muffle furnace, obtains TiO
2quantum-dot modified InVO
4particle;
Wherein, described polymer-type TiO
2the preparation method of colloidal sol is: it is 1.5～5 that butyl titanate is added to pH value, and in hydrochloric ethanol water, wherein the mol ratio of butyl titanate and water is 1: 4 mix the rear 2h of stirring, obtain polymer-type TiO
2colloidal sol, polymer-type TiO
2the solid content of colloidal sol regulates by the consumption of ethanol;
Step B: by the modification InVO making in steps A
4particle is distributed to and in ethanol water, obtains system, with hydrochloric acid, system pH is adjusted to 1.5～3, under the stirring in water bath condition of 50～80 ℃, to the mixed liquor that drips butyl titanate and absolute ethyl alcohol in this system, make the mol ratio of In and Ti reach 1: 20～1: 5, after dropwising, reaction 2h～10h, again by sedimentation and filtration, by least 3 post-dryings of absolute ethanol washing, obtain TiO
2/ InVO
4nano junction composite;
Wherein, modification InVO
4the solid content of particle in system is 10%～30%, and the mass fraction of ethanol water is 10%～50%, and in the mixed liquor of butyl titanate and absolute ethyl alcohol, the mass fraction of butyl titanate is 5%～50%.
As further improvement, in described steps A, join polymer-type TiO
2inVO in colloidal sol
4particle, particle diameter is 0.05 μ m～2 μ m.
As further improvement, in step B, when dripping the mixed liquor of butyl titanate and absolute ethyl alcohol in system, adopt the speed of 0.1mL/min～1mL/min at the uniform velocity to drip.
As further improvement, the modification InVO making in described steps A
4the TiO of particle surface
2quantum dot is discontinuous island and distributes.
Operation principle of the present invention: the present invention adopts sol-gel process, first passes through polymer-type colloidal sol at InVO
4particle surface forms the TiO that island distributes
2quantum dot, then utilizes butyl titanate to be fully hydrolyzed and obtains inorganic hydrate titanium ion [Ti (OH)
h(OH
2)
6-h]
(4-h)+, form TiO
2crystal growth unit, thereby by controlling growth unit with InVO
4the TiO of particle surface
2quantum dot is that core is grown, and prepares required TiO
2/ InVO
4nano junction material.
Compared with prior art, the invention has the beneficial effects as follows:
1, solve the forming core problem of nanocrystalline growth, avoided excessive coated formation nucleocapsid structure in traditional one-step method preparation process or nanocrystalline homogeneous phase in solution to separate out;
2, utilize hydrate titanium ion to solve nanocrystalline normal pressure liquid growth problem as growth unit, and tradition preparation all need pressurization or follow-up crystallization and thermal treatment;
3, prepared nano junction composite is by TiO
2and InVO
4all be exposed to material surface, when light induced electron is from InVO
4to TiO
2after migration, at TiO
2upper by enrichment electronics, and InVO
4on leave hole, thereby make surface show photocatalytic-oxidation voltinism and reproducibility simultaneously.
The specific embodiment
Below in conjunction with the specific embodiment, the present invention is described in further detail:
TiO
2/ InVO
4the preparation method of nano junction composite, comprises the following steps:
Steps A: be the InVO of 0.05 μ m～2 μ m by particle diameter
4it is 1%～5% polymer-type TiO that particle joins solid content
2in colloidal sol, and to make the mol ratio of In and Ti be 1: 50～1: 10, then after 50 ℃ of stirring in water bath 1h～10h, by sedimentation and filtration, obtain powders by 3 post-dryings of absolute ethanol washing, this powder is placed in to 350 ℃ of insulation 2h of Muffle furnace, obtains TiO
2quantum-dot modified InVO
4particle, the TiO on surface
2quantum dot is discontinuous island and distributes.
Wherein, described polymer-type TiO
2the preparation method of colloidal sol is: it is 1.5～5 that butyl titanate is added to pH value, and in hydrochloric ethanol water, wherein the mol ratio of butyl titanate and water is 1: 4, after mixing, stirs 2h, obtains polymer-type TiO
2colloidal sol, polymer-type TiO
2the solid content of colloidal sol carrys out regulation system by the consumption of ethanol.
Step B: by the modification InVO making in steps A
4particle is distributed to and in ethanol water, obtains system, with hydrochloric acid, system pH is adjusted to 1.5～3, under the stirring in water bath condition of 50～80 ℃, by the speed of 0.1mL/min～1mL/min at the uniform velocity to the mixed liquor that drips butyl titanate and absolute ethyl alcohol in this system, make the mol ratio of In and Ti reach 1: 20～1: 5, after dropwising, reaction 2h～10h, by sedimentation and filtration, 3 post-dryings of use absolute ethanol washing, obtain TiO again
2/ InVO
4nano junction composite;
Wherein, modification InVO
4the solid content of particle in system is 10%～30%, and the mass fraction of ethanol water is 10%～50%, and in the mixed liquor of butyl titanate and absolute ethyl alcohol, the mass fraction of butyl titanate is 5%～50%.
The following examples can make this professional professional and technical personnel's comprehend the present invention, but do not limit the present invention in any way.By 8 embodiment, successfully make TiO respectively
2/ InVO
4nano junction composite, the test data in each embodiment sees the following form 1.
Table 1 embodiment tables of data
Finally, it should be noted that above what enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above embodiment, can also have a lot of distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (4)
1.TiO
2/ InVO
4the preparation method of nano junction composite, is characterized in that, comprises the following steps:
Steps A: by InVO
4it is 1%～5% polymer-type TiO that particle joins solid content
2in colloidal sol, and to make the mol ratio of In and Ti be 1: 50～1: 10, then after 50 ℃ of stirring in water bath 1h～10h, by sedimentation and filtration, obtain powders by least 3 post-dryings of absolute ethanol washing, this powder is placed in to 350 ℃ of insulation 2h of Muffle furnace, obtains TiO
2quantum-dot modified InVO
4particle;
Wherein, described polymer-type TiO
2the preparation method of colloidal sol is: it is 1.5～5 that butyl titanate is added to pH value, and in hydrochloric ethanol water, wherein the mol ratio of butyl titanate and water is 1: 4, after mixing, stirs 2h, obtains polymer-type TiO
2colloidal sol, polymer-type TiO
2the solid content of colloidal sol regulates by the consumption of ethanol;
Step B: by the modification InVO making in steps A
4particle is distributed in ethanol water and obtains system, with hydrochloric acid by system
ph value is adjusted to 1.5～3, under the stirring in water bath condition of 50～80 ℃, to the mixed liquor that drips butyl titanate and absolute ethyl alcohol in this system, make the mol ratio of In and Ti reach 1: 20～1: 5, after dropwising, reaction 2h～10h, then by sedimentation and filtration, by least 3 post-dryings of absolute ethanol washing, obtain TiO
2/ InVO
4nano junction composite;
Wherein, modification InVO
4the solid content of particle in system is 10%～30%, and the mass fraction of ethanol water is 10%～50%, and in the mixed liquor of butyl titanate and absolute ethyl alcohol, the mass fraction of butyl titanate is 5%～50%.
2. TiO according to claim 1
2/ InVO
4the preparation method of nano junction composite, is characterized in that, joins polymer-type TiO in described steps A
2inVO in colloidal sol
4particle, particle diameter is 0.05 μ m～2 μ m.
3. TiO according to claim 1
2/ InVO
4the preparation method of nano junction composite, is characterized in that, in step B, when dripping the mixed liquor of butyl titanate and absolute ethyl alcohol in system, adopts the speed of 0.1mL/min～1mL/min at the uniform velocity to drip.
4. TiO according to claim 1
2/ InVO
4the preparation method of nano junction composite, is characterized in that, the modification InVO making in described steps A
4the TiO of particle surface
2quantum dot is discontinuous island and distributes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104096557A (en) * | 2014-07-29 | 2014-10-15 | 山东大学 | Preparation method of heterojunction type MVO4 and TiO2 composite photocatalysis fiber |
| CN105457621A (en) * | 2015-11-24 | 2016-04-06 | 李跃军 | Preparation method of heterojunction titanium dioxide/rare-earth doped vanadate composite nanofiber photocatalytic material |
| CN109901260A (en) * | 2019-04-28 | 2019-06-18 | 安徽帝显电子有限公司 | A kind of processing method of light guiding film |
| CN110697687A (en) * | 2019-10-25 | 2020-01-17 | 扬州昇业机械有限公司 | A1 with core-shell structure2O3Preparation method of coated CNTs powder |
| CN112915782A (en) * | 2021-01-27 | 2021-06-08 | 张娟丽 | Composite nano material for air purification and preparation method thereof |
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|---|---|---|---|---|
| CN102602997A (en) * | 2012-03-01 | 2012-07-25 | 长沙学院 | Method for preparing indium vanadate nano particles |
| CN103301846A (en) * | 2013-07-11 | 2013-09-18 | 中南大学 | InVO4.Cu2O.TiO2 ternary complex and preparation method and application thereof |
-
2013
- 2013-11-19 CN CN201310585798.6A patent/CN103599770B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602997A (en) * | 2012-03-01 | 2012-07-25 | 长沙学院 | Method for preparing indium vanadate nano particles |
| CN103301846A (en) * | 2013-07-11 | 2013-09-18 | 中南大学 | InVO4.Cu2O.TiO2 ternary complex and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| XUEJUN ZOU,ET AL: "Synthesis of LaVO4/TiO2 heterojunction nanotubes by sol-gel coupled with hydrothermal method for photocatalytic air purification", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
| YULIN MIN,ET AL: "Sonodegradation and photodegradation of methyl orange by InVO4/TiO2 nanojunction composites under ultrasonic and visible light irradiation", 《ULTRASONICS SONOCHEMISTRY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104096557A (en) * | 2014-07-29 | 2014-10-15 | 山东大学 | Preparation method of heterojunction type MVO4 and TiO2 composite photocatalysis fiber |
| CN104096557B (en) * | 2014-07-29 | 2016-02-03 | 山东大学 | Heterojunction type MVO 4with TiO 2the preparation method of composite photocatalyst fiber |
| CN105457621A (en) * | 2015-11-24 | 2016-04-06 | 李跃军 | Preparation method of heterojunction titanium dioxide/rare-earth doped vanadate composite nanofiber photocatalytic material |
| CN109901260A (en) * | 2019-04-28 | 2019-06-18 | 安徽帝显电子有限公司 | A kind of processing method of light guiding film |
| CN110697687A (en) * | 2019-10-25 | 2020-01-17 | 扬州昇业机械有限公司 | A1 with core-shell structure2O3Preparation method of coated CNTs powder |
| CN112915782A (en) * | 2021-01-27 | 2021-06-08 | 张娟丽 | Composite nano material for air purification and preparation method thereof |
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|---|---|
| CN103599770B (en) | 2015-08-26 |
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