CN108439462B - Preparation method of pyrochlore type rare earth titanate powder - Google Patents

Preparation method of pyrochlore type rare earth titanate powder Download PDF

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CN108439462B
CN108439462B CN201810262604.1A CN201810262604A CN108439462B CN 108439462 B CN108439462 B CN 108439462B CN 201810262604 A CN201810262604 A CN 201810262604A CN 108439462 B CN108439462 B CN 108439462B
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rare earth
powder
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sol
ethyl alcohol
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CN108439462A (en
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张乐
顾灵诚
邵岑
周天元
高光珍
王骋
陈浩
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XINYI DONGFANG SHUOHUA OPTICAL MATERIALS Co.,Ltd.
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    • C01G23/00—Compounds of titanium
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Abstract

The invention discloses a preparation method of pyrochlore type rare earth titanate powder, which is prepared by adopting a soft chemical sol-gel method and comprises the following specific steps: (1) respectively weighing rare earth nitrate powder and titanium alkoxide according to a stoichiometric ratio; (2) dissolving a rare earth nitrate raw material in absolute ethyl alcohol at room temperature to obtain a solution A; simultaneously adding acetylacetone and titanium alkoxide into absolute ethyl alcohol to obtain a solution B; mixing the solution A and the solution B to obtain transparent sol; dropwise adding a dilute nitric acid solution into the transparent sol at 40-60 ℃, continuously stirring, monitoring the pH value, stopping dropwise adding when the pH value is 4.0-5.0, and standing for 15-30 min to obtain a transparent wet gel; (3) drying the wet gel for 12-24 h at 100-120 ℃, and grinding to obtain powder; (4) and (3) placing the powder in a muffle furnace, and preserving heat for 2-4 h at the temperature of 750-850 ℃ to obtain pyrochlore type rare earth titanate powder. The invention has simple preparation process, low energy consumption, uniform chemical composition of the prepared powder and high product purity.

Description

Preparation method of pyrochlore type rare earth titanate powder
Technical Field
The invention belongs to the field of optical materials, relates to rare earth titanate, and particularly relates to a preparation method of pyrochlore type rare earth titanate powder.
Background
Rare earth titanate (RE)2Ti2O7) Is an important chemical product and has wide application and research in the fields of photovoltaic devices, photocatalysts, water purification, electrolyte and the like. The existing methods for synthesizing rare earth titanate mainly comprise a high-temperature solid-phase synthesis method, a sol-gel method, ultrasonic spray pyrolysis, pulse laser deposition and the like. Among them, the sol-gel method has been popular as one of the most suitable techniques for synthesizing rare earth titanate powder. However, when the sol-gel method is used to prepare titanate powder, the gelation rate of the sol is difficult to control, and ions cannot completely enter the network in the chemical reaction complexing process, so that the stoichiometric ratio is affected, and the preparation of pure-phase powder cannot be realized.
Disclosure of Invention
The invention aims to provide a preparation method of pyrochlore type rare earth titanate powder, which has the advantages of simple process, easy operation, short preparation period and uniform chemical composition of the prepared powder.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for preparing pyrochlore type rare earth titanate powder by adopting a soft chemical sol-gel method comprises the following specific steps:
(1) weighing: according to the general formula RE2Ti2O7Respectively weighing rare earth nitrate powder and titanium alkoxide according to the stoichiometric ratio of the elements, wherein the purity of the rare earth nitrate raw material is higher than 99.99%;
(2) sol gelation: dissolving a rare earth nitrate raw material in absolute ethyl alcohol at room temperature, wherein the mass volume ratio of the rare earth nitrate to the absolute ethyl alcohol is 0.1-0.5 mol: 1L, stirring for 20-30 min to obtain a solution A; adding acetylacetone and titanium alkoxide into absolute ethyl alcohol at room temperature, wherein the mass volume ratio of acetylacetone to absolute ethyl alcohol is 0.1-0.2 mol: 1L, the mass volume ratio of the titanium alkoxide to the absolute ethyl alcohol is 0.05-0.15 mol: 1L, stirring for 20-30 min to obtain a solution B; mixing the solution A and the solution B, and stirring for 10-15 min to obtain transparent sol; dripping 1-3 mol/L dilute nitric acid solution into the transparent sol, continuously stirring, monitoring the pH value, stopping dripping when the pH value is 4.0-5.0, standing for 15-30 min to obtain transparent wet gel, and keeping the temperature of the system at 40-60 ℃ in the sol-gel process;
(3) and (3) drying: placing the wet gel obtained in the step (2) in a drying oven, drying for 12-24 h at 100-120 ℃, and grinding to obtain powder;
(4) and (3) calcining: and (4) placing the powder obtained in the step (3) in a muffle furnace, and preserving heat for 2-4 hours at the temperature of 750-850 ℃ to obtain pure-phase pyrochlore type rare earth titanate powder.
Preferably, the rare earth nitrate is dysprosium nitrate or samarium nitrate.
Preferably, the titanium alkoxide is selected from titanium isopropoxide, tetrabutyl titanate, tetraisopropyl titanate or tetraethyl titanate. More preferably, the titanium alkoxide is titanium isopropoxide.
Preferably, the dropping speed of the dilute nitric acid solution in the step (2) is 1-5 drops/min.
Compared with the prior art, the invention has the beneficial effects that:
(1) the single-phase pyrochlore-structure rare earth titanate powder prepared by the soft sol-gel method is in the shape of nearly spherical particles, uniform in chemical composition, high in product purity and good in dispersity, and due to recombination of free excitons, a remarkable PL emission peak appears in the prepared rare earth titanate, so that the single-phase pyrochlore-structure rare earth titanate powder can be applied to manufacturing of devices such as photovoltaic devices, photocatalysts, water purification and electrolysis.
(2) Before adding the titanium dioxide precursor, the rare earth nitrate is dissolved in absolute ethyl alcohol to ensure the uniform distribution of rare earth ions; adding acetylacetone to a precursor of titanium dioxide to prevent precipitation of titanium dioxide; and the gel with better uniformity is obtained by adjusting the pH value of the sol system.
(3) The preparation method has the advantages of simple preparation process, economic raw materials, low energy consumption, low cost, suitability for industrial production, no industrial three wastes in the reaction process, and environmental protection.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1 preparation of Dy2Ti2O7
A process for preparing pyrochlore-type rare-earth titanate powder includes such steps as
(1) Weighing: according to the chemical formula Dy2Ti2O736.653g of dysprosium nitrate (Dy (NO3)3.xH2O) and 28.422g of titanium isopropoxide are respectively weighed according to the stoichiometric ratio of the elements, wherein the purity of the dysprosium nitrate is higher than 99.99 percent;
(2) sol gelation: dissolving a rare earth nitrate raw material in absolute ethyl alcohol at room temperature, wherein the mass volume ratio of the rare earth nitrate to the absolute ethyl alcohol is 0.1 mol: 1L, stirring for 20min to obtain solution A; ② simultaneously adding 1ml of acetylacetone and titanium isopropoxide into absolute ethyl alcohol at room temperature, wherein the mass volume ratio of the acetylacetone to the absolute ethyl alcohol is 0.1: 1L, the mass-volume ratio of titanium isopropoxide to absolute ethyl alcohol is 0.05 mol: 1L, stirring for 20min to obtain a solution B; mixing the solution A and the solution B, and stirring for 15min to obtain transparent sol; dripping 1mol/L dilute nitric acid solution into the transparent sol at the dripping speed of 5 drops/min, continuously stirring, monitoring the pH value, stopping dripping when the pH value is 4.0, standing for 15min to obtain transparent wet gel, and keeping the system temperature at 40 ℃ in the sol-gel process;
(3) and (3) drying: putting the wet gel obtained in the step (2) into a drying oven, drying for 24 hours at the temperature of 100 ℃, and grinding to obtain powder;
(4) and (3) calcining: and (4) placing the powder obtained in the step (3) in a muffle furnace, and preserving the heat for 4 hours at the temperature of 750 ℃ to obtain pure-phase pyrochlore type rare earth titanate powder.
The test results were as follows:
XRD analysis confirms that the synthesized powder is pyrochlore structure, TEM image shows that the particles are nearly spherical, and the average grain size is 35 nm. Under the excitation of 200nm ultraviolet light, strong 423nm wavelength blue-violet light is emitted.
EXAMPLE 2 preparation of Sm2Ti2O7
A process for preparing pyrochlore-type rare-earth titanate powder includes such steps as
(1) Weighing: according to the chemical formula Sm2Ti2O7133.335gg samarium nitrate (Sm (NO) is weighed according to the stoichiometric ratio of each element3)3.6H2O) and 85.266g of titanium isopropoxide, wherein the purity of dysprosium nitrate is higher than 99.99%;
(2) sol gelation: dissolving a rare earth nitrate raw material in absolute ethyl alcohol at room temperature, wherein the mass volume ratio of the rare earth nitrate to the absolute ethyl alcohol is 0.3 mol: 1L, stirring for 25min to obtain solution A; adding acetylacetone and titanium isopropoxide into absolute ethyl alcohol at room temperature, wherein the mass-volume ratio of acetylacetone to absolute ethyl alcohol is 0.15 mol: 1L, the mass-to-volume ratio of titanium isopropoxide to absolute ethyl alcohol is 0.1 mol: 1L, stirring for 25min to obtain a solution B; mixing the solution A and the solution B, and stirring for 12min to obtain transparent sol; dripping dilute nitric acid solution with the concentration of 2mol/L into the transparent sol at the dripping speed of 3 drops/min, continuously stirring, monitoring the pH value, stopping dripping when the pH value is 4.5, standing for 20min to obtain transparent wet gel, and keeping the system temperature at 50 ℃ in the sol-gel process;
(3) and (3) drying: putting the wet gel obtained in the step (2) into a drying oven, drying for 18h at the temperature of 110 ℃, and grinding to obtain powder;
(4) and (3) calcining: and (4) placing the powder obtained in the step (3) in a muffle furnace, and preserving the heat for 3 hours at the temperature of 800 ℃ to obtain pure-phase pyrochlore type rare earth titanate powder.
The test results were as follows:
XRD analysis confirms that the synthesized powder is pyrochlore structure, and TEM image shows that the particles are nearly spherical and the average grain size is 42 nm. Under the excitation of 200nm ultraviolet light, strong blue-violet light with 426nm wavelength is emitted.
Example 3 preparation of Dy2Ti2O7
A process for preparing pyrochlore-type rare-earth titanate powder includes such steps as
(1) Weighing: according to the chemical formula Dy2Ti2O7183.265g dysprosium nitrate (Dy (NO) was weighed out based on the stoichiometric ratio of each element3)3.xH2O) and 142.11g of titanium isopropoxide, wherein the purity of dysprosium nitrate is higher than 99.99%;
(2) sol gelation: dissolving a rare earth nitrate raw material in absolute ethyl alcohol at room temperature, wherein the mass volume ratio of the rare earth nitrate to the absolute ethyl alcohol is 0.5 mol: 1L, stirring for 30min to obtain a solution A; ② at room temperature, simultaneously adding 2ml of acetylacetone and titanium isopropoxide into absolute ethyl alcohol, the mass volume ratio of acetylacetone to absolute ethyl alcohol is 0.2 mol: 1L, the mass-to-volume ratio of titanium isopropoxide to absolute ethyl alcohol is 0.15 mol: 1L, stirring for 30min to obtain a solution B; mixing the solution A and the solution B, and stirring for 15min to obtain transparent sol; dripping dilute nitric acid solution with the concentration of 3mol/L into the transparent sol at the dripping speed of 1 drop/min, continuously stirring, monitoring the pH value, stopping dripping when the pH value is 5.0, standing for 15-30 min to obtain transparent wet gel, and keeping the system temperature at 60 ℃ in the sol-gel process;
(3) and (3) drying: putting the wet gel obtained in the step (2) into a drying oven, drying for 12h at 120 ℃, and grinding to obtain powder;
(4) and (3) calcining: and (4) placing the powder obtained in the step (3) in a muffle furnace, and preserving heat for 2 hours at the temperature of 850 ℃ to obtain pure-phase pyrochlore type rare earth titanate powder.
The test results were as follows:
XRD analysis confirmed that the synthesized powder is pyrochlore structure, TEM image shows that the particles are nearly spherical, and the average grain size is 68 nm. Under the excitation of 200nm ultraviolet light, the blue-violet light with stronger 423nm wavelength is emitted.
The above-mentioned embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above-mentioned embodiments, and any other modifications, substitutions, combinations, and simplifications which are made without departing from the spirit and principle of the present invention are all equivalent replacements within the protection scope of the present invention.

Claims (1)

1. A method for preparing pyrochlore type rare earth titanate powder is characterized by adopting a soft chemical sol-gel method for preparation, and the specific preparation steps are as follows:
(1) weighing: according to the general formula RE2Ti2O7Respectively weighing rare earth nitrate powder and titanium isopropoxide according to the stoichiometric ratio of the elements, wherein the purity of the rare earth nitrate raw material is higher than 99.99%, and the rare earth nitrate is dysprosium nitrate or samarium nitrate;
(2) sol gelation: dissolving a rare earth nitrate raw material in absolute ethyl alcohol at room temperature, wherein the ratio of the amount of a rare earth nitrate substance to the volume of the absolute ethyl alcohol is 0.1-0.5 mol: 1L, stirring for 20-30 min to obtain a solution A; adding acetylacetone and titanium isopropoxide into absolute ethyl alcohol at room temperature, wherein the ratio of the amount of acetylacetone to the volume of absolute ethyl alcohol is 0.1-0.2 mol: 1L, the volume ratio of the titanium isopropoxide substance to the absolute ethyl alcohol is 0.05-0.15 mol: 1L, stirring for 20-30 min to obtain a solution B; mixing the solution A and the solution B, and stirring for 10-15 min to obtain transparent sol; dripping 1-3 mol/L dilute nitric acid solution into the transparent sol, continuously stirring, monitoring the pH value, stopping dripping when the pH value is 4.0-5.0, standing for 15-30 min to obtain transparent wet gel, and keeping the temperature of the system at 40-60 ℃ in the sol-gel process;
(3) and (3) drying: placing the wet gel obtained in the step (2) in a drying oven, drying for 12-24 hours at 100-120 ℃, and grinding to obtain powder;
(4) and (3) calcining: and (4) placing the powder obtained in the step (3) in a muffle furnace, and preserving heat for 2-4 hours at the temperature of 750-850 ℃ to obtain pure-phase pyrochlore type rare earth titanate powder.
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