CN103395837A - Preparation method of Bi12TiO20 powder - Google Patents

Abstract

The invention relates to a preparation method of Bi12TiO20 powder. The preparation method comprises the following steps of: adding NaOH into deionized water and stirring till dissolution; respectively weighing Bi(NO3)3.5H2O and TiO2 according to the Bi/Ti ion molar ratio of 12: 1, adding into a NaOH solution and stirring to obtain a precursor solution which is uniformly mixed; transferring the precursor solution into a microwave reaction kettle; placing the microwave reaction kettle into a microwave hydrothermal reaction device for reacting; and cooling after the end of reaction, taking out of the reaction kettle, firstly washing an obtained product with distilled water to be neutral, then washing with anhydrous ethanol, and finally drying in an oven to obtain the Bi12TiO20 powder. According to the preparation method disclosed by the invention, a microwave hydrothermal method is adopted for preparing the Bi12TiO20 powder, the adopted process is simple, the efficiency is high, and the obtained powder has the advantages of complete development of crystal phase, high purity, regular grain morphology and uniform size.

Description

Bi 12TiO 20The preparation method of powder

Technical field

The invention belongs to field of functional materials, particularly a kind of Bi ₁₂TiO ₂₀The preparation method of powder.

Background technology

Bi ₁₂TiO ₂₀Be a kind of in the numerous oxide compounds of bismuth titanates series, its crystalline structure is isometric system 123 point groups, and structure cell is by [TiO ₄] tetrahedron and [BiO ₅] two structural units compositions of polyhedron.Bi ₁₂TiO ₂₀Have the advantages such as specific rotation is little, linear electro-optic coefficient large, red light district sensitivity height, belong to broadband semiconductor, it has the character such as photoelectricity, electric light, fluorescence, magneto-optic, acousto-optic, optically-active and piezoelectricity simultaneously.Particularly its good photoelectricity and electrooptical property, make it in fields such as photoelectron, optics, optical information processing materials, extremely wide application prospect be arranged.The crystalline structure that the Bismuth Titanate-based Ferroelectrics compound is peculiar and electronic structure make them have the performance of semiconductor light-catalyst, and research finds that their band-gap energy is 2.6～2.8eV, all less than TiO ₂Band-gap energy, so this compounds has photo-catalysis capability under visible light, Bi wherein ₁₂TiO ₂₀Photocatalytic activity the strongest, almost reached and P-25(TiO ₂) identical activity.

At present, Bi ₁₂TiO ₂₀The synthetic method of powder mainly contains coprecipitation method and chemical solution decomposition method.But these two kinds of methods need high-temperature calcination, and the gained powder is easily reunited, and pattern is difficult to control.Microwave-hydrothermal method is a kind of method of new synthetic powder, and it combines traditional hydrothermal synthesis method and microwave field, has given full play to the advantage of microwave and hydrothermal method.The characteristics such as it is fast that microwave-hydrothermal method has speed of response, and the product granularity is controlled and purity is high, better crystallinity degree, reunion are few, brought into play in recent years great advantage and had vast potential for future development in the preparation of inorganic ceramic powder material.

Summary of the invention

, in order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of Bi ₁₂TiO ₂₀The preparation method of powder, adopt microwave-hydrothermal method to prepare Bi ₁₂TiO ₂₀Powder, the technique that adopts is simple, efficiency is high, and gained powder crystalline phase is grown complete, and purity is high; Grain morphology rule, size uniform.

To achieve these goals, the technical solution used in the present invention is:

A kind of Bi ₁₂TiO ₂₀The preparation method of powder, comprise the steps:

Step 1: NaOH is joined in deionized water, be stirred to dissolving, the concentration of NaOH is 1.0～3.0mol/L;

Step 2: by Bi, Ti ion mol ratio 12:1, take respectively Bi (NO ₃) ₃5H ₂O and TiO ₂, and join in NaOH solution, stirring the precursor liquid that obtains mixing after 0.5～1h, in precursor liquid, Bi, Ti total ion concentration are 0.01～0.10mol/L;

Step 3: precursor liquid is changed in microwave reaction kettle, and the volume of precursor liquid is controlled at the 50%-70% of microwave reaction kettle volume;

Step 4: microwave reaction kettle is put into the microwave hydrothermal conversion unit, allow precursor liquid react 30～120min under 150～220 ℃;

Step 5: question response finish cooling after, take out reactor, use again absolute ethanol washing 1 time after products therefrom first is washed with distilled water to neutrality,, finally by oven drying, obtain Bi ₁₂TiO ₂₀Powder.

Compared with prior art, the present invention adopts microwave-hydrothermal method, has synthesized Bi ₁₂TiO ₂₀Powder.Processing method of the present invention is simple, efficiency is high, be convenient to doping; Owing to not needing follow-up calcination processing, the good dispersity of powder; In addition, gained powder crystalline phase is grown complete, and purity is high, pattern rule, size uniform, tiny.Bi ₁₂TiO ₂₀The microwave hydrothermal of powder synthesizes its preparation a kind of new route is provided, and is expected to also promote that people carry out more deep structure research to aspects such as its properities.

Description of drawings

Fig. 1 is the XRD figure spectrum of the powder of the embodiment of the present invention three preparations.

Fig. 2 is the Bi of the embodiment of the present invention three preparations ₁₂TiO ₂₀The SEM figure of powder.

Embodiment

Describe embodiments of the present invention in detail below in conjunction with drawings and Examples.

Embodiment one

A kind of Bi ₁₂TiO ₂₀The preparation method of powder, comprise the steps:

Step 1: NaOH is joined in deionized water, be stirred to dissolving, the concentration of NaOH is 1.0mol/L;

Step 2: by Bi, Ti ion mol ratio 12:1, take respectively Bi (NO ₃) ₃5H ₂O and TiO ₂, and join in NaOH solution, stirring the precursor liquid that obtains mixing after 0.5h, in precursor liquid, Bi, Ti total ion concentration are 0.01mol/L;

Step 3: precursor liquid is changed in microwave reaction kettle, and the volume of precursor liquid is controlled at 50% of microwave reaction kettle volume;

Step 4: microwave reaction kettle is put into the microwave hydrothermal conversion unit, allow precursor liquid react 120min under 150 ℃;

Step 5: question response finish cooling after, take out reactor, use again absolute ethanol washing 1 time after products therefrom first is washed with distilled water to neutrality,, finally by oven drying, obtain Bi ₁₂TiO ₂₀Powder.

Embodiment two

A kind of Bi ₁₂TiO ₂₀The preparation method of powder, comprise the steps:

Step 1: NaOH is joined in deionized water, be stirred to dissolving, the concentration of NaOH is 3.0mol/L;

Step 2: by Bi, Ti ion mol ratio 12:1, take respectively Bi (NO ₃) ₃5H ₂O and TiO ₂, and join in NaOH solution, stirring the precursor liquid that obtains mixing after 1h, in precursor liquid, Bi, Ti total ion concentration are 0.10mol/L;

Step 3: precursor liquid is changed in microwave reaction kettle, and the volume of precursor liquid is controlled at 70% of microwave reaction kettle volume;

Step 4: microwave reaction kettle is put into the microwave hydrothermal conversion unit, allow precursor liquid react 30min under 220 ℃;

Step 5: question response finish cooling after, take out reactor, use again absolute ethanol washing 1 time after products therefrom first is washed with distilled water to neutrality,, finally by oven drying, obtain Bi ₁₂TiO ₂₀Powder.

Embodiment three

A kind of Bi ₁₂TiO ₂₀The preparation method of powder, comprise the steps:

Step 1: NaOH is joined in deionized water, be stirred to dissolving, the concentration of NaOH is 2.0mol/L;

Step 2: by Bi, Ti ion mol ratio 12:1, take respectively Bi (NO ₃) ₃5H ₂O and TiO ₂, and join in NaOH solution, stirring the precursor liquid that obtains mixing after 0.8h, in precursor liquid, Bi, Ti total ion concentration are 0.06mol/L;

Step 3: precursor liquid is changed in microwave reaction kettle, and the volume of precursor liquid is controlled at 60% of microwave reaction kettle volume;

Step 4: microwave reaction kettle is put into the microwave hydrothermal conversion unit, allow precursor liquid react 80min under 180 ℃;

Step 5: question response finish cooling after, take out reactor, use again absolute ethanol washing 1 time after products therefrom first is washed with distilled water to neutrality,, finally by oven drying, obtain Bi ₁₂TiO ₂₀Powder.

Fig. 1 is the XRD figure spectrum of the powder of preparation, can find out that the standard card NO.78-1158 in itself and PDF database fits like a glove, and illustrates that the crystalline phase of powder consists of Bi ₁₂TiO ₂₀, the peak type at visible X-ray diffraction peak is sharp-pointed in addition, peak is higher by force, illustrates that the powder crystal formation physically well develops.Fig. 2 is the Bi of preparation ₁₂TiO ₂₀The SEM figure of powder, visible powder granule is better dispersed, and the pattern rule, like spherical; Particle size is even in addition, is about 100nm.

Claims (1)

1. Bi ₁₂TiO ₂₀The preparation method of powder, is characterized in that, comprises the steps:

Step 1: NaOH is joined in deionized water, be stirred to dissolving, the concentration of NaOH is 1.0～3.0mol/L;

Step 2: by Bi, Ti ion mol ratio 12:1, take respectively Bi (NO ₃) ₃5H ₂O and TiO ₂, and join in NaOH solution, stirring the precursor liquid that obtains mixing after 0.5～1h, in precursor liquid, Bi, Ti total ion concentration are 0.01～0.10mol/L;

Step 3: precursor liquid is changed in microwave reaction kettle, and the volume of precursor liquid is controlled at the 50%-70% of microwave reaction kettle volume;

Step 4: microwave reaction kettle is put into the microwave hydrothermal conversion unit, allow precursor liquid react 30～120min under 150～220 ℃;

Step 5: question response finish cooling after, take out reactor, use again absolute ethanol washing 1 time after products therefrom first is washed with distilled water to neutrality,, finally by oven drying, obtain Bi ₁₂TiO ₂₀Powder.

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