CN103601239A - Preparation method of anatase and brookite mixed crystal TiO2 nanowire - Google Patents
Preparation method of anatase and brookite mixed crystal TiO2 nanowire Download PDFInfo
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- CN103601239A CN103601239A CN201310592566.3A CN201310592566A CN103601239A CN 103601239 A CN103601239 A CN 103601239A CN 201310592566 A CN201310592566 A CN 201310592566A CN 103601239 A CN103601239 A CN 103601239A
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Abstract
The invention discloses a preparation method of an anatase and brookite mixed crystal TiO2 nanowire, and belongs to the technical field of TiO2 nanometer materials. The preparation method comprises the following steps: adding anatase and brookite mixed crystal P25 particles into a NaOH solution, carrying out ultrasound treatment, uniformly stirring and mixing, carrying out hydrothermal reaction for 24-48 hours when the temperature of a mixed solution is 180-200 DEG C, then naturally cooling to a room temperature, washing a reaction product with deionized water until the reaction product is neutral, stirring and washing with HCI (Hydrochloric acid), then washing with deionized water until the mixture is neutral, drying in air, finally heating the product to 500-550 DEG C at a certain rate and calcining, thus obtaining the anatase and brookite mixed crystal TiO2 nanowire. The preparation method has the advantages that the preparation technology is simple, and the prepared anatase and brookite mixed crystal TiO2 nanowire contains anatase crystal forms and brookite crystal forms and has good photocatalysis performance.
Description
Technical field
The present invention relates to the mixed crystal TiO of a kind of anatase octahedrite and brookite
2the preparation method of nano wire, belongs to TiO
2technical field of nano material.
Background technology
In the modern life, energy shortage and environmental pollution become the problem that people pay special attention to.Photocatalitic Technique of Semiconductor can directly utilize sun power to realize water decomposition to prepare clean energy hydrogen, decomposing organic pollutant or CO2 is reduced into hydrocarbon fuels, thereby is considered to effectively to solve the green method of energy environment issues.In numerous photocatalyst materials, TiO
2due to its at a low price, nontoxic, stable chemical nature, catalytic activity is good, oxidation capacity advantages of higher obtains people common concern, for TiO
2research be also the focus in this field always.
The photocatalytic activity of semiconductor material is determined by many factors such as the crystal formation, lattice defect, degree of crystallinity, material specific surface area of material conventionally jointly, and wherein crystal formation is an extremely important factor.TiO
2have three kinds of crystal formations: anatase octahedrite, rutile and brookite.Detitanium-ore-type TiO
2energy gap be 3.2 eV, there is good photocatalytic activity; Rutile TiO
2energy gap be 3.0 eV, ultraviolet ray is had to good shielding effect and chemical stability; Brookite type TiO
2structure is stable not, so Detitanium-ore-type TiO
2and rutile TiO
2the most frequently used TiO
2, for example Degussa P25 is the mixed crystal type TiO that the ratio of Anatase and Rutile Type is approximately 4:1
2, be also most widely used mixed crystal TiO
2product.Aspect photochemical catalysis, mixed crystal TiO
2exist " Mixed crystal effect ", the active TiO that often surpasses monocrystalline phase
2.
Prepare at present mixed crystal TiO
2one of method be vapor phase process, P25 for example; Other method is mainly with TiCl
4or tetrabutyl titanate is raw material, adopt the method for sol-gel or hydro-thermal, the TiO preparing
2mostly be the mixed phase of rutile and two kinds of crystal formations of anatase octahedrite, and pattern is mostly nano particle.
Summary of the invention
The object of the present invention is to provide a kind of anatase octahedrite and brookite mixed crystal TiO
2the preparation method of nano wire, this preparation method's process is simple, the TiO of prepared anatase octahedrite and brookite mixed crystal
2nano wire has higher photocatalysis performance.
The present invention is achieved by the following technical solutions, a kind of anatase octahedrite and brookite mixed crystal TiO
2the preparation method of nano wire, is characterized in that comprising following process:
NaOH is dissolved in to deionized water, and compound concentration is the NaOH solution of 8～12 mol/L, pressing NaOH in solution is 16:1 with the P25 granular mass ratio of anatase octahedrite and rutile-type mixed crystal, the P25 particle of anatase octahedrite and rutile-type mixed crystal is joined in NaOH solution, through ultrasonic, be uniformly mixed, mixing solutions is carried out under 180～200 ℃ of conditions to hydro-thermal reaction 24～48 h, then naturally cool to room temperature, reaction product is extremely neutral with deionized water wash, by concentration, be after the HCl agitator treating of 0.1 mol/L again, extremely neutral with deionized water wash, after air drying, product is risen to 500～550 ℃ of calcining 3 h with the speed of 5 ℃/min, obtain the TiO of anatase octahedrite and brookite mixing crystal formation
2nano wire.
The present invention has the following advantages: preparation technology is simple, the TiO of preparation
2nano wire contains brookite and two kinds of crystal formations of anatase octahedrite, the TiO of this mixed crystal
2nano wire has good photocatalysis performance.
Accompanying drawing explanation
Fig. 1 is the prepared TiO of embodiment mono-
2the SEM figure of nano wire.
Fig. 2 is the prepared TiO of embodiment mono-
2the TEM figure of nano wire.
Fig. 3 is the prepared TiO of embodiment mono-
2the XRD figure of nano wire.
In figure: ■ represents anatase octahedrite composition; ▲ represent brookite composition.
Embodiment
Below in conjunction with example, the present invention will be further described, and these examples, just for the present invention is described, do not limit the present invention.
Embodiment mono-
Prepare the NaOH solution that 80 mL concentration are 10 mol/L; Take the P25 powder of 2 g anatase octahedrites and rutile mixed crystal, join in NaOH solution, ultrasonic 30 min, stir 30 min, and solution mixes; Subsequently the solution preparing is transferred in hydrothermal reaction kettle, put into baking oven at 200 ℃ of reaction 24 h; After hydro-thermal reaction finishes, product in reactor is washed till to neutrality with deionized water, by product stirring and pickling 5 h in the hydrochloric acid soln of 0.1 mol/L, with deionized water, product is washed till to neutrality more subsequently, in air, dry, finally product is warming up to 500 ℃ of calcining 3 h with 5 ℃/min, obtains the TiO of anatase octahedrite and brookite mixed crystal
2nano wire.
Embodiment bis-
The present embodiment is identical with embodiment mono-step, and difference is: the P25 powder quality taking is become to 2.4 g from 2 g, and the hydro-thermal reaction time becomes 48 h from 24 h.
Embodiment tri-
The present embodiment is identical with embodiment mono-step, and difference is: hydrothermal temperature is become to 180 ℃ from 200 ℃, and the hydro-thermal reaction time becomes 48 h from 24 h, and calcining temperature becomes 550 ℃ from 500 ℃.
Embodiment tetra-
The present embodiment is identical with embodiment mono-step, and difference is: the stirring and pickling time in the hydrochloric acid at 0.1 mol/L is become to 3 h from 5 h, and calcination time becomes 2 h from 3 h.
Claims (1)
1. an anatase octahedrite and brookite mixed crystal TiO
2the preparation method of nano wire, is characterized in that comprising following process:
It is the NaOH solution of 8～12 mol/L that NaOH powder is joined to compound concentration in deionized water, pressing NaOH in solution is 16:1 with the P25 granular mass ratio of anatase octahedrite and rutile-type mixed crystal, the P25 particle of anatase octahedrite and rutile-type mixed crystal is joined in NaOH solution, through ultrasonic, be uniformly mixed, mixing solutions is 180～200 ℃ in temperature and carries out hydro-thermal reaction 24～48 h, then naturally cool to room temperature, reaction product is extremely neutral with deionized water wash, by concentration, be after the HCl agitator treating of 0.1 mol/L, extremely neutral with deionized water wash, then at air drying, finally product is risen to 500～550 ℃ of calcining 3 h with the speed of 5 ℃/min, obtain the TiO of anatase octahedrite and brookite mixing crystal formation
2nano wire.
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| CN201310592566.3A CN103601239A (en) | 2013-11-22 | 2013-11-22 | Preparation method of anatase and brookite mixed crystal TiO2 nanowire |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525168A (en) * | 2014-12-18 | 2015-04-22 | 黑龙江大学 | Method for synthesizing anatase/brookite nano composite material for photocatalytic decomposition of water into hydrogen through one-step hydrothermal method |
| CN105776327A (en) * | 2016-03-25 | 2016-07-20 | 武汉理工大学 | Nanorod-assembled type brookite and anatase mixed-phase TiO2 micrometer hollow sphere and preparation method and application thereof |
| CN106975488A (en) * | 2016-01-15 | 2017-07-25 | 上海乐泽环境工程有限公司 | It is a kind of that aluminium-nano-TiO is activated with Ni-2For the efficient elctro-catalyst of active centre |
| CN108097225A (en) * | 2017-11-23 | 2018-06-01 | 昆明理工大学 | A kind of method that crystal type nano TiO 2 is prepared using seed crystal induction |
| CN111617760A (en) * | 2020-06-29 | 2020-09-04 | 盐城工学院 | Mn-TiO2Composite photocatalytic material and preparation method and application thereof |
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| CN1613585A (en) * | 2004-11-09 | 2005-05-11 | 北京航空航天大学 | Method for preparing titania wiring pipe and use for wiring pipe |
| CN101920990A (en) * | 2010-07-23 | 2010-12-22 | 上海师范大学 | Method for preparing titanium dioxide nanowires by adopting high-pressure microwave method |
| CN102774882A (en) * | 2012-07-05 | 2012-11-14 | 常州大学 | Method for preparing candied haw-shaped pure anatase type nano-titania wire in larger scale |
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2013
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| CN1613585A (en) * | 2004-11-09 | 2005-05-11 | 北京航空航天大学 | Method for preparing titania wiring pipe and use for wiring pipe |
| CN101920990A (en) * | 2010-07-23 | 2010-12-22 | 上海师范大学 | Method for preparing titanium dioxide nanowires by adopting high-pressure microwave method |
| CN102774882A (en) * | 2012-07-05 | 2012-11-14 | 常州大学 | Method for preparing candied haw-shaped pure anatase type nano-titania wire in larger scale |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525168A (en) * | 2014-12-18 | 2015-04-22 | 黑龙江大学 | Method for synthesizing anatase/brookite nano composite material for photocatalytic decomposition of water into hydrogen through one-step hydrothermal method |
| CN106975488A (en) * | 2016-01-15 | 2017-07-25 | 上海乐泽环境工程有限公司 | It is a kind of that aluminium-nano-TiO is activated with Ni-2For the efficient elctro-catalyst of active centre |
| CN105776327A (en) * | 2016-03-25 | 2016-07-20 | 武汉理工大学 | Nanorod-assembled type brookite and anatase mixed-phase TiO2 micrometer hollow sphere and preparation method and application thereof |
| CN105776327B (en) * | 2016-03-25 | 2017-09-29 | 武汉理工大学 | A kind of brockite and anatase mixed phase TiO of nanometer rods assembling2Micrometre hollow sphere and its preparation method and application |
| CN108097225A (en) * | 2017-11-23 | 2018-06-01 | 昆明理工大学 | A kind of method that crystal type nano TiO 2 is prepared using seed crystal induction |
| CN108097225B (en) * | 2017-11-23 | 2021-05-14 | 昆明理工大学 | Method for preparing crystal form nano titanium dioxide by seed crystal induction |
| CN111617760A (en) * | 2020-06-29 | 2020-09-04 | 盐城工学院 | Mn-TiO2Composite photocatalytic material and preparation method and application thereof |
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Application publication date: 20140226 |